CN113502453B - High-reflection nano film and preparation method and application thereof - Google Patents

High-reflection nano film and preparation method and application thereof Download PDF

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CN113502453B
CN113502453B CN202110811822.8A CN202110811822A CN113502453B CN 113502453 B CN113502453 B CN 113502453B CN 202110811822 A CN202110811822 A CN 202110811822A CN 113502453 B CN113502453 B CN 113502453B
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thickness
refractive index
index layer
sio
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CN113502453A (en
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于海亮
朱斌
陈小群
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Lens Technology Changsha 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
    • C23C14/10—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
    • C23C14/0694—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
    • C23C14/08—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
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • 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
    • 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
    • C23C14/24—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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
    • G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/08—Mirrors
    • G02B5/0808—Mirrors having a single reflecting layer
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/285—Interference filters comprising deposited thin solid films
    • H—ELECTRICITY
    • H04—ELECTRIC COMMUNICATION TECHNIQUE
    • H04M—TELEPHONIC COMMUNICATION
    • H04M1/00—Substation equipment, e.g. for use by subscribers
    • H04M1/02—Constructional features of telephone sets
    • H04M1/0202—Portable telephone sets, e.g. cordless phones, mobile phones or bar type handsets
    • H04M1/0279—Improving the user comfort or ergonomics
    • H04M1/0283—Improving the user comfort or ergonomics for providing a decorative aspect, e.g. customization of casings, exchangeable faceplate
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention provides a high-reflection nano film and a preparation method and application thereof, and relates to the technical field of coating, wherein the film comprises a base material, a transition layer with the thickness of 10-30nm, a first high refractive index layer with the thickness of 6-15nm, a first low refractive index layer with the thickness of 65-80nm, a second high refractive index layer with the thickness of 50-65nm, a second low refractive index layer with the thickness of 10-90nm, a metal layer with the thickness of 25-90nm and a third low refractive index layer with the thickness of 25-70nm which are arranged in sequence from bottom to top; the ratio of the sum of the thicknesses of the second low refractive index layer and the third low refractive index layer to the thickness of the metal layer is 1: (1-3); the thickness of the high-reflection nano film is less than or equal to 440 nm. The invention can achieve the reflection effect of more than or equal to 95 percent under the condition of thinner film thickness, and the coating layer meets the reliability requirement and meets the individualized requirement of customers on the visual effect of the surface appearance of the ceramic, the glass or the gem.

Description

High-reflection nano film and preparation method and application thereof
Technical Field
The invention relates to the technical field of coating, in particular to a high-reflection nano film and a preparation method and application thereof.
Background
With the popularization of smart phones, the requirements of consumers on the appearance of the smart phones are higher and higher, the back covers of the smart phones made of non-metal materials become one of the design directions pursued by high-end models of most consumer electronics manufacturers at present, the highly-reflective brightening color films are the most mainstream design schemes at present, and in the coming years, the back covers of the smart phones are gradually changed from metal materials to non-metal materials represented mainly by ceramics, glass and jewels. The appearance effect, scratch resistance and the like formed on the surface of the ceramic, glass or gem only by adopting the traditional silk-screen or metal coating technology cannot meet the requirement of confidence tolerance, and the preparation process has the trouble of high reflection and dazzle color and seriously influences the aesthetic effect of appearance, so the preparation process of the high reflection nano film with strong scratch resistance, high adhesive force and high reflection has great application value.
At present, the coating film on the surface of the non-metal material is difficult to achieve the effect of dazzling colors in high reflection, in order to achieve the effect of dazzling colors in high reflection, materials with high refractive index and low refractive index are overlapped in the prior art, and the interference effect principle of light is utilized to achieve the effect of high reflection, for example, patent CN111747658A discloses a dazzling color-changing coated glass, which comprises a glass substrate and an outer layer Nb with high refractive index2O5Film layer of high refractive index Nb from glass substrate to outer layer2O5A plurality of inner layers of high-refractive-index Nb are sequentially and alternately arranged in the direction of the film layer2O5Film layer, inner layer low refractive index SiO2The total thickness of the film layer is 1500nm, so that the high-reflection colorful film obtained by superposition (the thickness needs to be 1500nm to achieve a high-reflection effect) is too thick, the adhesive force is not strong, and the performances of poaching in hundreds of grids cannot meet the requirements.
In addition, in the prior art, a metal layer is directly plated on the surface of the film layer, but the metal plated material is easy to conduct, seriously interferes with equipment signals such as a mobile phone and the like, and has a color influence effect.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
One of the purposes of the invention is to provide a high-reflection nano film, which can achieve a high standard reflection effect with the reflection of more than or equal to 95% under the condition of a thinner film, and a plating layer meets the reliability requirement and meets the individualized requirement of customers on the surface appearance visual effect of ceramics, glass or gemstones (3D, 2.5D, plain film).
The second objective of the present invention is to provide a method for preparing a highly reflective nano-film.
The third object of the present invention is to provide an application of the high reflective nano thin film.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
in a first aspect, the invention provides a high-reflection nano film, which comprises a substrate, a transition layer, a first high refractive index layer, a first low refractive index layer, a second high refractive index layer, a second low refractive index layer, a metal layer and a third low refractive index layer which are arranged from bottom to top in sequence;
the metal layer comprises an aluminum layer, an indium layer or a silver layer;
the thickness of the transition layer is 10-30 nm;
the thickness of the first high refractive index layer is 6-15 nm;
the thickness of the first low refractive index layer is 65-80 nm;
the thickness of the second high refractive index layer is 50-65 nm;
the thickness of the second low refractive index layer is 10-90 nm;
the thickness of the metal layer is 25-90 nm;
the thickness of the third low refractive index layer is 25-70 nm;
the ratio of the sum of the thicknesses of the second low refractive index layer and the third low refractive index layer to the thickness of the metal layer is 1: (1-3);
the thickness of the high-reflection nano film is less than 440 nm.
Further, the transition layer comprises SiO2Layer or SiO2And Al2O3And a mixed layer.
Further, the first high refractive index layer and the second high refractive index layer each independently include TiO2Layer, Nb2O5One of the layers.
Further, the first low refractive index layer, the second low refractive index layer, and the third low refractive index layer each independently include SiO2A layer, a magnesium fluoride layer, or a silicon aluminum oxide layer.
Further, the high-reflection nano film comprises a base material and SiO with the thickness of 10-30nm which are arranged from bottom to top in sequence2Layer of TiO with thickness of 6-15nm2Layer of SiO with thickness of 65-80nm2Layer of TiO 50-65nm thick2Layer of SiO with thickness of 60-75nm2A layer, an Al layer with a thickness of 60-75nm and SiO with a thickness of 25-45nm2And (3) a layer.
Further, the high-reflection nano film comprises a nano film and a nano film layer sequentially arranged from bottom to topA substrate, SiO with a thickness of 10-30nm2Layer of TiO 6-9nm thick2Layer of SiO with thickness of 64-72nm2Layer of TiO with thickness of 55-65nm2Layer of SiO with thickness of 52-65nm2A layer, an indium layer with a thickness of 45-55nm and SiO with a thickness of 25-45nm2And (3) a layer.
Further, the substrate is ceramic, glass or gem stone.
In a second aspect, the invention provides a method for preparing the high-reflection nano film, which comprises the following steps:
and depositing a transition layer, a first high refractive index layer, a first low refractive index layer, a second high refractive index layer, a second low refractive index layer, a metal layer and a third low refractive index layer on the substrate in sequence to obtain the high-reflection nano film.
Further, a deposition coating is carried out by adopting an evaporation coating or magnetron sputtering method.
In a third aspect, the invention provides an application of the high-reflection nano film in preparing a cover plate of an electronic product.
The invention has at least the following beneficial effects:
according to the invention, through the high and low refractive index layers and the metal layers which are alternately arranged and the reasonable matching and arrangement of the material, the position and the thickness of each layer, not only is a high standard reflection effect of more than or equal to 95% of reflection achieved under the condition of the thickness of the thin film layer, but also the thin film has good binding force and meets the requirements on resistance and reliability.
The invention is suitable for the high-reflection coating on the surfaces of glass, jewels, ceramics and PET substrates, and achieves the effect of dazzling colors in appearance.
The preparation method has high efficiency and high yield.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a measured reflection diagram of a high reflection nano-film obtained in example 1 of the present invention;
FIG. 2 is a measured reflection diagram of the highly reflective nano-film obtained in comparative example 1 of the present invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the prior art, the non-metal surface is coated with a film to achieve the effect of high reflection and colorful; the film layer that can achieve the high-reflection dazzling effect is too thick.
The invention provides a high-reflection nano film made of a metal material, which is used for solving the problem of high-reflection colorful surface of the existing transparent ceramic material, transparent glass or gem, so as to meet the individual requirements of customers on the visual effect of the surface of the ceramic, glass or gem (3D, 2.5D or flat sheet), and can achieve the high-standard reflection effect with the reflection of more than or equal to 95% under the condition of a thicker film, and the coating layer meets the reliability requirement.
The high-reflection nano film comprises a base material, a transition layer, a first high-refractive-index layer, a first low-refractive-index layer, a second high-refractive-index layer, a second low-refractive-index layer, a metal layer and a third low-refractive-index layer which are sequentially arranged from bottom to top;
the high reflection here means that the reflectance of the film is not less than 95%.
The substrate herein mainly refers to a non-metal substrate such as ceramic, glass, or gem stone.
The film of the present invention comprises essentially seven layers. The first transition layer mainly plays a role in improving the adhesive force between the base material (glass) and the film; the transition layer material includes, but is not limited to, silica, or a mixture of silica and alumina, with silica being preferred. The thickness of the transition layer is 10-30nm, such as 10, 15, 20, 25, 30 nm.
The second layer to the fifth layer are used for adjusting color and reflection, and the color and reflection of the film are adjusted by adjusting the film thickness of 2-5 layers according to the light wave curve.
The second layer of the first high refractive index layer material is a high refractive index material, and the high refractive index material generally refers to a material with a refractive index of 1.65 or more, including but not limited to titanium dioxide, niobium pentoxide, and the like, and preferably titanium dioxide. The thickness of the first high refractive index layer is 6-15nm, for example 6, 7, 8, 9, 10, 11, 12, 13, 14, 15 nm.
The third layer of the first low refractive index layer material is a low refractive index material, where the low refractive index material generally refers to a material having a refractive index of less than 1.65, including but not limited to silicon dioxide, magnesium fluoride, silicon aluminum oxide, and the like. The thickness of the first low refractive index layer is 65-80nm, such as 68, 70, 72, 75, 78, 80 nm.
The fourth layer of the second high refractive index layer material is a high refractive index material, and the high refractive index material generally refers to a material with a refractive index of 1.65 or more, including but not limited to titanium dioxide, niobium pentoxide, and the like, and preferably titanium dioxide. The thickness of the second high refractive index layer is 50-65nm, such as 52, 55, 58, 60, 62 nm.
The fifth layer of the second low refractive index layer material is a low refractive index material, where the low refractive index material generally refers to a material having a refractive index of less than 1.65, including but not limited to silicon dioxide, magnesium fluoride, silicon aluminum oxide, and the like. The thickness of the second low refractive index layer is 10-90nm, such as 15, 20, 25, 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85 nm.
The sixth metal layer is used for improving the reflectivity and achieving the effect of dazzling, but has an influence on the color of the film, so that the metal needs to be selected. The metal layer is an aluminum layer, an indium layer or a silver layer; the thickness of the metal layer is 25-90nm, such as 30, 35, 40, 45, 50, 55, 60, 65, 70, 75, 80, 85 or 90 nm.
The seventh layer of the third low refractive index layer is used for protecting the film layer and increasing the resistance, and the material of the third low refractive index layer is a low refractive material, where the low refractive material generally refers to a material with a refractive index less than 1.65, and includes but is not limited to silicon dioxide, magnesium fluoride, silicon aluminum oxide, and the like. The thickness of the third low refractive index layer is 25-70nm, e.g. 25, 30, 35, 40, 45, 50, 55, 60, 65, 70 nm.
The ratio of the sum of the thicknesses of the second low refractive index layer and the third low refractive index layer to the thickness of the metal layer is 1: (1-3), for example, 1: 1. 1: 2. 1: 3;
the total thickness of the high-reflection nano film is less than 440 nm.
The surface of the film layer is directly plated with a metal layer, the product is conductive, and can seriously interfere equipment signals of a mobile phone and the like, low-refractive-index layers (silicon dioxide layers) are added in the front and the back of the metal layer to isolate the conductivity, the resistance is actually measured to be about 50G omega, the resistance is measured to be about 40 omega without adding the low-refractive-index layers (silicon dioxide layers), and the mobile phone signals can not be influenced when the resistance standard value of a client side is required to be more than 400 omega.
The metal layer metal of the invention is selected from metals with high reflection and silvery white characteristics, such as aluminum, indium, silver and the like. Metals with weak reflectivity can not achieve high reflection effect, such as pure metal titanium and the like, the pure metal titanium replaces aluminum or indium, and the measured reflection value is only 47.8% and is blue, so that the high reflection effect can not be achieved.
According to the invention, the metal layer is arranged on the sixth layer, and 2-5 layers of the high refractive index layer (titanium dioxide) and the low refractive index layer (silicon dioxide) are plated in front of the metal layer for the purpose of enhancing reflection and adjusting color, if the metal layer (aluminum) is arranged on the second layer, the measured reflection is 85%, the reflection effect is only 85.4% when the metal layer (aluminum) is arranged on the third layer, and the color and the reflection effect of the high refractive index layer (titanium dioxide) and the low refractive index layer (silicon dioxide) plated behind the metal layer (aluminum) cannot penetrate through the metal layer (aluminum), so that the high reflection effect cannot be achieved.
The thickness of the metal layer ranges from 25nm to 90nm, the first layer must be plated with a transition layer (silicon dioxide) and has a thickness of 10nm to 30nm, the first layer (fifth layer) before the metal layer must be plated with a low refractive index layer (silicon dioxide) and has a thickness of 10nm to 90nm, the second layer (seventh layer) after the metal layer is plated with a low refractive index layer (silicon dioxide) and has a thickness of 25nm to 70nm, and the thickness of the metal layer: the combined thickness of the fifth layer and the seventh layer is (1-3): 1, so can effectively promote the rete cohesion, resistance and reliability problem, because fifth layer and seventh layer membrane thickness are too thin, fifth layer low refractive index layer (silica) thickness 5nm, resistance NG, when adjusting thickness to 10nm, test result ok, seventh layer low refractive index layer (silica) 20nm, resistant hand sweat and resistance test NG, when promoting thickness to 25nm, test result ok, fifth layer and seventh layer membrane layer are too thick influences this scheme and originally reduces the original intention of membrane thickness under the circumstances of keeping high reflectivity, in addition the restriction metal layer thickness: the combined thickness of the fifth layer and the seventh layer is (1-3): 1 is to satisfy the requirement of resistance, because the thickness of the metal layer is increased and the corresponding insulating layer is changed.
Therefore, the high-refractive-index and low-refractive-index metal layers and the metal layers are alternately arranged, and the materials, positions and thicknesses of the layers are reasonably matched and arranged, so that the high-standard reflection effect is achieved, the thinning design is realized, and the film has good bonding force and meets the requirements on resistance and reliability.
In a preferred embodiment, the high-reflection nano film comprises a substrate and SiO with the thickness of 10-30nm which are arranged from bottom to top in sequence2Layer of TiO with thickness of 6-15nm2Layer of SiO with thickness of 65-80nm2Layer of TiO 50-65nm thick2Layer of SiO with thickness of 60-75nm2A layer, an Al layer with a thickness of 60-75nm and SiO with a thickness of 25-45nm2And (3) a layer.
In another preferred embodiment, the high-reflection nano film comprises a substrate and SiO with the thickness of 10-30nm which are arranged in sequence from bottom to top2Layer of TiO 6-9nm thick2Layer of SiO with thickness of 64-72nm2Layer of TiO with thickness of 55-65nm2Layer of SiO with thickness of 52-65nm2A layer, an indium layer with a thickness of 45-55nm and SiO with a thickness of 25-45nm2And (3) a layer.
The invention also provides a preparation method of the high-reflection nano film, which comprises the following steps:
and depositing a transition layer, a first high refractive index layer, a first low refractive index layer, a second high refractive index layer, a second low refractive index layer, a metal layer and a third low refractive index layer on the substrate in sequence to obtain the high-reflection nano film.
The plating method is not limited, and evaporation, magnetron sputtering, or the like may be used.
Specifically, the preparation method of the typical high-reflection nano film comprises the following steps:
1. cleaning a ceramic, glass or gem (3D, 2.5D, plain film) substrate by using an ultrasonic cleaner, sticking and fixing the front by using a protective film, and taking the back as an area to be coated with a film;
2. placing the base material for checking OK on an umbrella of the evaporator cavity, fixing the base material by using a magnet, closing the machine, exhausting air, and selecting a designed program to coat the film;
3. the preparation process parameters of the high-reflection nano film of the aluminum material are as follows:
3.1 both the sputter and the evaporator can realize high reflection effect, but preferably adopts an evaporation coating machine, and adopts aluminum, oxygen, a crucible and common materials with high and low refractive index (silicon dioxide and titanium dioxide);
3.2 coating parameters: the ion source is clean, the first layer of silicon dioxide is 10-30nm, the second layer of titanium dioxide is 6-15nm, the third layer of silicon dioxide is 65-80nm, the fourth layer of titanium dioxide is 50-65nm, the fifth layer of silicon dioxide is 60-75nm, the sixth layer of aluminum is 60-75nm, and the seventh layer of silicon dioxide is 25-45 nm.
Aluminum materials are susceptible to oxidation resulting in reduced reflection. If oxygen is filled during coating, the aluminum oxide is changed into aluminum oxide, and no ion source auxiliary coating is added during aluminum plating, so that no gas is required to be filled, and if ion source auxiliary coating is required, inert gas (argon) is filled.
The metal aluminum may be replaced with metal indium, with the following parameters: 10-30nm of first layer silicon dioxide, 6-9nm of second layer titanium dioxide, 64-72nm of third layer silicon dioxide, 55-65nm of fourth layer titanium dioxide, 52-65nm of fifth layer silicon dioxide, 45-55nm of sixth layer indium and 25-45nm of seventh layer silicon dioxide.
The invention also provides an application of the high-reflection nano film in the preparation of an electronic product cover plate.
Electronic products include, but are not limited to, smart phones, tablet computers, electronic watches, and the like. The method can be used for preparing the rear cover of the smart phone, and meets the requirement of consumers on the appearance of the smart phone.
The invention is further illustrated by the following examples. The materials in the examples are prepared according to known methods or are directly commercially available, unless otherwise specified.
Example 1
In the embodiment, a 3D product of a glass sheet with the thickness of 152.22 +/-0.08 multiplied by 73.94 +/-0.08 multiplied by 0.6 +/-0.02 mm is prepared, and the preparation process of the high-reflection nano film of the aluminum material is carried out according to the following specific process steps:
1. preparing a high-gloss polished glass product, cleaning the glass product by adopting a full-automatic twelve-groove ultrasonic cleaning machine, and pasting the glass product on a plate to prepare film coating;
2. sticking and fixing the front surface of a glass substrate by using a protective film, wherein the back surface is an area to be coated, and the sprayed ink is black ink which meets the requirement of a signal tolerance test;
3. the pasted product is placed on an umbrella of a Dinghua 2350 evaporation coating machine and fixed by a magnet, and the coating steps are as follows:
3.1 putting the coating materials of silicon dioxide/titanium dioxide and the like into a crucible, closing the door and vacuumizing;
3.2 evacuation to 3.0X 10-3Clicking to start film coating after Pa;
3.2.1 plasma clean, parameters as follows:
Figure BDA0003168604760000091
3.2.2 first layer Silica (SiO)2)：
Figure BDA0003168604760000092
3.2.3 second layer of titanium dioxide (TiO)2)：
Figure BDA0003168604760000093
3.2.4 third layer of Silica (SiO)2)：
Figure BDA0003168604760000094
3.2.5 fourth layer of titanium dioxide (TiO)2)：
Figure BDA0003168604760000101
3.2.6 fifth layer Silica (SiO)2)：
Figure BDA0003168604760000102
3.2.7 sixth layer aluminum (Al):
Figure BDA0003168604760000103
3.2.8 layer seven Silica (SiO)2)：
Figure BDA0003168604760000104
And (5) performing ink spraying treatment on the sample subjected to film coating.
The measured reflectance of the sample is shown in FIG. 1, the wavelength is between 420 and 680nm of visible light, and the measured reflectance is more than 95%.
The sample color was specular silver.
The results of the plating reliability are shown in the following table:
Figure BDA0003168604760000111
example 2
Example 2 differs from example 1 in that the film layers differ in thickness: first layer of silicon dioxide (SiO)215nm), second layer of titanium dioxide (TiO)210nm), third layer of silicon dioxide (SiO)275nm), fourth layer of titanium dioxide (TiO)2,60nm)，Fifth layer of silicon dioxide (SiO)260nm), a sixth layer of aluminum (Al,75nm), a seventh layer of silicon dioxide (SiO)240nm), a reflectance of 95.2% was measured, and the color was pale blue.
Example 3
Example 3 differs from example 1 in that the metal layer and the film layers differ in thickness: first layer of silicon dioxide (SiO)215nm), second layer of titanium dioxide (TiO)26nm), third layer of silicon dioxide (SiO)268nm), fourth layer of titanium dioxide (TiO)260nm), fifth layer of silicon dioxide (SiO)258nm), a sixth layer of indium (In,50nm), a seventh layer of silicon dioxide (SiO)240nm), the reflectance was measured to be 95.3%, and the color specular silver.
The results of the plating reliability are shown in the following table:
Figure BDA0003168604760000112
Figure BDA0003168604760000121
example 4
Example 4 differs from example 3 in that the film layers differ in thickness: first layer of silicon dioxide (SiO)230nm), second layer of titanium dioxide (TiO)29nm), third layer of silicon dioxide (SiO)264nm), fourth layer of titanium dioxide (TiO)265nm), fifth layer of silicon dioxide (SiO)252nm), a sixth layer of indium (In,45nm), a seventh layer of silicon dioxide (SiO)225nm), a reflectance of 95% was measured, and the color was pale blue.
Comparative example 1
Superposition of titanium dioxide and silicon dioxide:
film layer 1 2 3 4 5 6 7 8
Material SiO2 TiO2 SiO2 TiO2 SiO2 TiO2 SiO2 TiO2
1/4 optical thickness 0.8017 0.3613 0.8870 0.5503 0.8959 0.8654 0.8671 0.7246
Physical thickness (nm) 75.77 20.83 83.82 31.72 84.66 49.89 91.94 41.78
Film layer 9 10 11 12 13 14 15 16
Material SiO2 TiO2 SiO2 TiO2 SiO2 TiO2 SiO2 TiO2
1/4 optical thickness 0.7588 0.8348 1.0208 1.1533 1.0841 1.0039 1.1433 1.1633
Physical thickness (nm) 71.71 48.13 96.47 66.49 102.45 57.88 108.05 67.07
Film layer 17 18 19 20 21
Material SiO2 TiO2 SiO2 TiO2 SiO2
1/4 optical thickness 1.1595 1.1700 1.3257 1.2157 0.7068
Physical thickness (nm) 109.48 67.45 125.28 70.09 66.79
The actual coating thickness is 1527 nm;
the measured reflection was 95%, as shown in FIG. 2.
The results of the plating reliability are shown in the following table:
Figure BDA0003168604760000131
therefore, the high-reflection colorful film obtained by superposing the materials with high refractive index and low refractive index is too thick, so that the adhesive force is not strong, and the performances of poaching in hundreds of grids and the like cannot meet the requirements.
Comparative example 2
The comparative example differs from example 1 in that the thickness of the second titanium dioxide film was adjusted to 30nm, the other films were unchanged, the measured reflectance was 92.8%, and the color was blue.
Comparative example 3
The comparative example is different from example 1 in that no silica layer is added before and after aluminum plating, i.e., the fifth layer and the seventh layer are omitted, and the thicknesses of other film layers are unchanged, so that the resistance is found to be not satisfactory, and the measured resistance is about 40 Ω.
Comparative example 4
This comparative example differs from example 1 in that aluminum was replaced with titanium and the other film layers were unchanged in thickness. The measured reflection value is only 47.8 percent and is blue, and the high reflection effect cannot be achieved.
Comparative example 5
The comparative example is different from example 1 in that the second layer is an aluminum layer, the second to fifth layers of example 1 are replaced with third to sixth layers, and the thicknesses of the other layers are unchanged, and the reflection is measured to be 85%.
Comparative example 6
The present comparative example is different from example 1 in that the aluminum layer is on the third layer, the third to fifth layers of example 1 are changed to the fourth to sixth layers, the other layers are unchanged, and the thickness is unchanged, and the reflection effect is only 85.4%.
Therefore, the metal layer (aluminum) cannot be penetrated by the high-refractive-index layer (titanium dioxide) and the low-refractive-index layer (silicon dioxide) plated behind the metal layer (aluminum) and the reflection effect, and the high reflection effect cannot be achieved.
Comparative example 7
The comparative example differs from example 1 in that the fifth silicon dioxide film thickness was adjusted to 5nm, and the other film thicknesses were not changed, resulting in a resistance NG.
Comparative example 8
This comparative example differs from example 1 in that the thickness of the seventh silica film layer was adjusted to 20nm, and the thickness of the other film layers was unchanged, resulting in resistance to hand perspiration and NG in the resistance test.
Comparative example 9
The difference between the comparative example and the example 1 is that the thickness of the sixth aluminum layer is adjusted to 15nm, the thickness of other film layers is unchanged, and the measured reflectivity is 78%, so that the high reflection effect cannot be achieved.
Comparative example 10
The difference between the comparative example and the example 1 is that the client requires the resistance to be greater than 400 Ω, the thickness of the fifth layer is 5nm, the thickness of the metal layer is 90nm, and the thickness of the seventh layer is 20nm, the measured resistance is about 150 Ω, and when the client does not meet the resistance requirements, the measured resistance is about 700 Ω when the thickness of the fifth layer is 10nm, the thickness of the metal layer is 90nm, and the thickness of the seventh layer is 25nm, and the test result is ok.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. A high-reflection nano film is characterized by comprising a base material, a transition layer, a first high-refractive-index layer, a first low-refractive-index layer, a second high-refractive-index layer, a second low-refractive-index layer, a metal layer and a third low-refractive-index layer which are sequentially arranged from bottom to top;
the metal layer comprises an aluminum layer, an indium layer or a silver layer;
the thickness of the transition layer is 10-30 nm;
the thickness of the first high refractive index layer is 6-15 nm;
the thickness of the first low refractive index layer is 65-80 nm;
the thickness of the second high refractive index layer is 50-65 nm;
the thickness of the second low refractive index layer is 10-90 nm;
the thickness of the metal layer is 25-90 nm;
the thickness of the third low refractive index layer is 25-70 nm;
the ratio of the sum of the thicknesses of the second low refractive index layer and the third low refractive index layer to the thickness of the metal layer is 1: (1-3);
the thickness of the high-reflection nano film is less than or equal to 440 nm.
2. The highly reflective nanofilm of claim 1, wherein the transition layer comprises SiO2Layer or SiO2And Al2O3And a mixed layer.
3. The highly reflective nanofilm of claim 1, wherein the first and second high refractive index layers each independently comprise TiO2Layer, Nb2O5One of the layers.
4. The high reflection nano-film according to claim 1, wherein the first low refractive index layer, the second low refractive index layer and the third low refractive index layer each independently comprise SiO2A layer, a magnesium fluoride layer, or a silicon aluminum oxide layer.
5. The high-reflection nano-film according to any one of claims 1 to 4, which comprises a substrate and SiO with a thickness of 10-30nm arranged in sequence from bottom to top2Layer of TiO with thickness of 6-15nm2Layer of SiO with thickness of 65-80nm2Layer of TiO 50-65nm thick2Layer of SiO with thickness of 60-75nm2A layer, an Al layer with a thickness of 60-75nm and SiO with a thickness of 25-45nm2And (3) a layer.
6. The high-reflection nano-film according to any one of claims 1 to 4, which comprises a substrate and SiO with a thickness of 10-30nm arranged in sequence from bottom to top2Layer of TiO 6-9nm thick2Layer of SiO with thickness of 64-72nm2Layer of TiO with thickness of 55-65nm2Layer of SiO with thickness of 52-65nm2A layer, an indium layer with a thickness of 45-55nm and SiO with a thickness of 25-45nm2And (3) a layer.
7. The high reflection nano-film according to any one of claims 1 to 4, wherein the substrate is ceramic, glass or gem stone.
8. The method for preparing the high-reflection nano film according to any one of claims 1 to 7, which comprises the following steps:
and depositing a transition layer, a first high refractive index layer, a first low refractive index layer, a second high refractive index layer, a second low refractive index layer, a metal layer and a third low refractive index layer on the substrate in sequence to obtain the high-reflection nano film.
9. The method according to claim 8, wherein the deposition coating is performed by evaporation or magnetron sputtering.
10. Use of a highly reflective nano-film according to any one of claims 1 to 7 for the production of cover sheets for electronic products.
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