CN113817986A - Coating material and preparation method thereof - Google Patents

Coating material and preparation method thereof Download PDF

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Publication number
CN113817986A
CN113817986A CN202010566202.8A CN202010566202A CN113817986A CN 113817986 A CN113817986 A CN 113817986A CN 202010566202 A CN202010566202 A CN 202010566202A CN 113817986 A CN113817986 A CN 113817986A
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China
Prior art keywords
layer
film layer
thickness
sio
film
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CN202010566202.8A
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Chinese (zh)
Inventor
李超
刘玉阳
黎原
王继厚
马兰
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BYD Co Ltd
Shantou BYD Electronics Co Ltd
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BYD Co Ltd
Shantou BYD Electronics Co Ltd
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Priority to CN202010566202.8A priority Critical patent/CN113817986A/en
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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
    • C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
    • 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
    • C23C14/08—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
    • C23C14/10—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
    • C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
    • C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon 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
    • C23C14/06—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
    • C23C14/06—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
    • C23C14/20—Metallic material, boron or silicon on organic substrates
    • C23C14/205—Metallic material, boron or silicon on organic 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
    • C23C14/46—Sputtering by ion beam produced by an external ion source
    • 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
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/285—Interference filters comprising deposited thin solid films

Abstract

In order to solve the problems that coating effects of coatings on different materials are seriously differentiated and optical constants are difficult to accurately debug in the prior art, the invention provides a coating material which comprises a base material, an Nb layer and a color layer, wherein the Nb layer is formed on the surface of the base material, the color layer is formed on the surface, deviating from the base material, of the Nb layer, the thickness of the Nb layer is larger than or equal to 140nm, the color layer comprises a plurality of low-refraction layers and a plurality of high-refraction layers, and the low-refraction layers and the high-refraction layers are alternately laminated. Meanwhile, the invention also discloses a preparation method of the coating material. The coating material provided by the invention can avoid the influence of the optical characteristics of different substrates on the optical parameters of the final coating, and achieves the purpose of adjustable color.

Description

Coating material and preparation method thereof
Technical Field
The invention belongs to the technical field of material coating, and particularly relates to a coating material and a preparation method thereof.
Background
The optical coating process is applied to products with high transmittance and small absorption materials in most cases. The optical coating technology is based on the principle of light interference, that is, light with different wavelengths interferes with the surface of the film, between the films and between the film and the substrate to achieve specific reflection or transmittance of light with specific wavelength on the substrate. It is required that the optical constants (reflectance, transmittance, extinction coefficient, etc.) of the substrate be measurable and stable.
If the coating process is applied to other various opaque materials, the limitations of the coating process brought by the above conditions are as follows:
1. different substrate materials have different optical characteristics, and if the same color or reflection effect is to be achieved, different film series film layers need to be redesigned and debugged again in mass production.
2. In order to ensure the touch feeling of common metal materials in electronic products, the surface roughness of the common metal materials is often much larger than that of glass products, and the large roughness fluctuation range can cause the color instability after the common metal materials are matched with a film layer.
3. The ceramic, metal and partial organic materials cannot be accurately fitted with respective optical constants, so that a plurality of colors cannot be realized through coating, namely, no adjustability exists.
Disclosure of Invention
The invention provides a coating material and a preparation method thereof, aiming at the problems of serious coating effect differentiation and difficulty in accurately debugging optical constants of coatings on different materials in the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
on one hand, the invention provides a coating material which comprises a base material, an Nb layer and a color layer, wherein the Nb layer is formed on the surface of the base material, the color layer is formed on the surface, away from the base material, of the Nb layer, the thickness of the Nb layer is larger than or equal to 140nm, the color layer comprises a plurality of low-refraction layers and a plurality of high-refraction layers, and the low-refraction layers and the high-refraction layers are alternately laminated.
Optionally, the thickness of the Nb layer is 140nm to 500 nm.
Optionally, the substrate comprises one or more of a ceramic, glass, metal, and organic material.
Optionally, the refractive index of the low refractive layer is less than 1.75, and the refractive index of the high refractive layer is greater than 1.9.
Optionally, the low refractive layer comprises SiO2、MgF2、Al2O3One or more of (a).
Optionally, the high refractive layer comprises Nb2O5、Si3N4、TiO2、Ti3O5And ZrO.
Optionally, the low refractive layer is selected from SiO2The high refractive layer is selected from Nb2O5。
Optionally, the thickness of the single layer of the low refractive layer is 5-400 nm, and the thickness of the single layer of the high refractive layer is 5-400 nm.
Optionally, the color layer sequentially includes a first Nb in a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2A film layer, whereinFirst Nb2O5The thickness of the film layer is 25-29 nm, and the first SiO is2The thickness of the film layer is 17-23 nm, and the second Nb is2O5The thickness of the film layer is 35-39 nm, and the second SiO is2The thickness of the film layer is 57-63 nm, and the third Nb is2O5The thickness of the film layer is 98-102 nm, and the third SiO is2The thickness of the film layer is 28-34 nm.
Optionally, the color layer sequentially includes a first Nb in a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 34-38 nm, and the first SiO layer2The thickness of the film layer is 82-88 nm, and the second Nb is2O5The thickness of the film layer is 79-84 nm, and the second SiO is2The thickness of the film layer is 127-133 nm, and the third Nb2O5The thickness of the film layer is 76-80 nm, and the third SiO is2The thickness of the film layer is 63-69 nm.
Optionally, the color layer sequentially includes a first SiO layer along a direction departing from the Nb layer2Film layer, first Nb2O5Film layer, second SiO2Film layer, second Nb2O5A film layer, wherein the first SiO2The thickness of the film layer is 71-77 nm, and the first Nb2O5The thickness of the film layer is 52-56 nm, and the second SiO is2The thickness of the film layer is 84-90 nm, and the second Nb is2O5The thickness of the film layer is 51-55 nm.
Optionally, the color layer sequentially includes a first Nb in a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 33-37 nm, and the first SiO layer2The thickness of the film layer is 73-79 nm, and the second Nb is2O5The thickness of the film layer is 71-75 nm, and the second SiO is2The thickness of the film layer is 137-143 nm, and the third Nb2O5The thickness of the film layer is 52-56 nm, and the third SiO is2The thickness of the film layer is 137-143 nm, and the fourth Nb is2O5The thickness of the film layer is 74-78 nm, and the fourth SiO is2The thickness of the film layer is 224-230 nm.
Optionally, the color layer sequentially includes a first Nb in a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 49-53 nm, and the first SiO layer2The thickness of the film layer is 93-99 nm, and the second Nb is2O5The thickness of the film layer is 54-58 nm, and the second SiO is2The thickness of the film layer is 63-69 nm, and the third Nb2O5The thickness of the film layer is 19-23 nm, and the third SiO is2The thickness of the film layer is 80-86 nm, and the fourth Nb is2O5The thickness of the film layer is 47-51 nm, and the fourth SiO is2The thickness of the film layer is 110-116 nm.
In another aspect, the present invention provides a method for preparing the coating material, comprising the following steps:
placing the substrate under a vacuum condition, bombarding the Nb target by adopting an ion source, depositing and forming an Nb layer on the surface of the substrate, and controlling the thickness of the Nb layer to be more than or equal to 140 nm;
and bombarding a target corresponding to the high-refraction layer and a target corresponding to the low-refraction layer by ions on the basis of the Nb layer and introducing auxiliary gas to form the high-refraction layer and the low-refraction layer which are alternated on the Nb layer.
According to the coating material provided by the invention, the simple substance Nb layer is formed on the surface of the base material to effectively cover the base material, and the final optical constant of the coating can be calculated by combining the refractive indexes of the low-refraction layer and the high-refraction layer in the color layer, so that the purpose of color regulation and control is achieved; when the thickness of the Nb layer is larger than 140nm, the reflected light reaches 50%, the provided reflected light is strong, the problem of dark color can be reduced, the covering effect is achieved, the influence of the optical characteristics of different base materials on the optical parameters of the final coating can be avoided, the color values of the coating films on different base materials are consistent, and the problem that the coating film color debugging difficulty is large due to the fact that the opaque base materials cannot accurately obtain the optical constants is solved. If the thickness of the Nb layer is too small, the effect of shielding is difficult to be obtained.
Drawings
FIG. 1 is a schematic structural diagram of a coating material provided in example 1 of the present invention;
FIG. 2 is a schematic structural diagram of a coating material provided in example 2 of the present invention;
FIG. 3 is a schematic structural diagram of a coating material provided in example 3 of the present invention;
FIG. 4 is a schematic structural diagram of a coating material provided in example 4 of the present invention;
FIG. 5 is a schematic structural diagram of a coating material provided in example 5 of the present invention;
FIG. 6 is a schematic structural view of a coating material provided in example 6 of the present invention;
FIG. 7 is a reflectance curve of the coating materials prepared in examples 1 to 3 of the present invention;
FIG. 8 is a reflectance curve of a plating material prepared in comparative example 1 of the present invention;
FIG. 9 is a reflectance curve of the plating material prepared in comparative example 2 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, an embodiment of the present invention provides a plating material, including a substrate, an Nb layer, and a color layer, where the Nb layer is formed on a surface of the substrate, the color layer is formed on a surface of the Nb layer facing away from the substrate, a thickness of the Nb layer is greater than or equal to 140nm, and the color layer includes a plurality of low-refractive layers and a plurality of high-refractive layers, where the plurality of low-refractive layers and the plurality of high-refractive layers are alternately stacked.
The surface of the substrate is covered effectively by forming the simple substance Nb layer, and the final optical constant of the coating can be calculated by combining the refractive indexes of the low-refraction layer and the high-refraction layer in the color layer, so that the purpose of color regulation and control is achieved; when the thickness of the Nb layer is larger than 140nm, the reflected light is up to 50%, the provided reflected light is strong, the problem of dark color can be reduced, the covering effect is achieved, the influence of the optical characteristics of different base materials on the optical parameters of the final coating can be avoided, the color values of the coating films on different base materials are consistent, and the problem that the coating film color debugging difficulty is large due to the fact that the opaque base materials cannot accurately obtain the optical constants is solved. If the thickness of the Nb layer is too small, the effect of shielding is difficult to be obtained.
By adopting the coating material provided by the invention, different base materials are replaced under the design of the same color layer and the same Nb layer, the embodied apparent colors are the same, namely the color values of the coating material on different base materials are consistent and are not influenced by the base materials. Therefore, when different substrates are produced, different film systems do not need to be debugged for different substrates, and different substrates can be placed in the same furnace of the same machine to complete film coating.
In some embodiments, the Nb layer has a thickness of 140nm to 500 nm.
The inventors have found through extensive experiments that the Nb layer performs the most shielding effect when the thickness thereof is between the above thickness ranges, and if the thickness of the Nb layer is excessively large, the cost of mass production increases, and it does not substantially contribute to color stability.
In some embodiments, the substrate comprises one or more of a ceramic, glass, metal, and organic material.
The organic material is preferably a resin material including one or more of Polyamide (PA), polybutylene terephthalate (PBT), Polycarbonate (PC), and polyphenylene sulfide (PPS).
The metal can adopt various metal simple substances or alloy materials, including copper, iron, aluminum, nickel and other metal simple substances and alloys thereof.
In a more preferred embodiment, the substrate is a spliced composite of different materials.
Because the optical properties of different materials of the spliced composite material are different, if a conventional film coating mode is adopted, obvious chromatic aberration occurs between different material areas, so that the appearance of the spliced composite material is influenced, and the boundary of the different material areas is obvious; when the coating material provided by the invention is applied to the spliced composite material, the influence of different materials in the spliced composite material on coating chromatic aberration can be shielded through the Nb layer, so that the spliced composite material shows the effect of consistent overall color.
In some embodiments, the low refractive layer has a refractive index of less than 1.75 and the high refractive layer has a refractive index of greater than 1.9.
Through the alternate lamination between the low refraction layer and the high refraction layer, light after being reflected by the Nb layer can form selective wavelength absorption, so that only light with specific wavelength is reflected to enter human eyes finally, and different color changes can be presented through the change of the refractive indexes, the quantity and the thicknesses of the low refraction layer and the high refraction layer.
Specifically, the thickness and the refractive index of each low-refractive layer may be set to be the same or different, and the thickness and the refractive index of each high-refractive layer may be set to be the same or different.
The color of the coating material is represented by a Lab color model, the wide adjustable range of the color can be realized by the matching of the Nb layer and the color layer, and specifically, the L value can be adjusted between 27 and 93; the value of a can be adjusted between-102 and 69; the b value can be adjusted between-109 and 110, thereby realizing the film forming effect of most colors.
In some embodiments, the low refractive layer comprises SiO2、MgF2、Al2O3One or more of (a).
In some embodiments, the high refractive layer comprises Nb2O5、Si3N4、TiO2、Ti3O5And ZrO.
In a more preferred embodiment, the low refractive layer is selected from SiO2The high refractive layer is selected from Nb2O5。
Compared with other low-refractive-index materials, SiO is selected2As a low refraction layer, the coating has the advantages of excellent acid and alkali resistance and strong adhesive force; compared with other high-refractive-index materials, Nb is selected2O5The high refractive layer has an advantage of a high film formation rate.
In some embodiments, the substrate is a metal substrate and the high refractive layer is selected from Nb2O5The high-refraction layer is in direct contact with the Nb layer, the Nb layer is made of a metal material and has good bonding strength with the metal base material, and meanwhile, the Nb layer and the Nb layer are in direct contact2O5The metal substrate, the Nb layer and the color layer have good affinity, and the bonding strength among the metal substrate, the Nb layer and the color layer can be effectively ensured.
In some embodiments, the thickness of the low refractive layer is 5 to 400nm, and the thickness of the high refractive layer is 5 to 400 nm.
As a preferred embodiment of the present invention, a yellow-green plating material is provided, which includes a substrate, an Nb layer and a color layer, wherein the Nb layer is formed on a surface of the substrate, the color layer is formed on a surface of the Nb layer away from the substrate, a thickness of the Nb layer is 140nm to 500nm, and the color layer sequentially includes a first Nb layer and a second Nb layer along a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2A film layer, whereinFirst Nb2O5The thickness of the film layer is 25-29 nm, and the first SiO is2The thickness of the film layer is 17-23 nm, and the second Nb is2O5The thickness of the film layer is 35-39 nm, and the second SiO is2The thickness of the film layer is 57-63 nm, and the third Nb is2O5The thickness of the film layer is 98-102 nm, and the third SiO is2The thickness of the film layer is 28-34 nm.
As a preferred embodiment of the present invention, a red plating material is provided, which includes a substrate, an Nb layer and a color layer, wherein the Nb layer is formed on a surface of the substrate, the color layer is formed on a surface of the Nb layer away from the substrate, a thickness of the Nb layer is 140nm to 500nm, and the color layer sequentially includes a first Nb layer and a second Nb layer along a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 34-38 nm, and the first SiO layer2The thickness of the film layer is 82-88 nm, and the second Nb is2O5The thickness of the film layer is 79-84 nm, and the second SiO is2The thickness of the film layer is 127-133 nm, and the third Nb2O5The thickness of the film layer is 76-80 nm, and the third SiO is2The thickness of the film layer is 63-69 nm.
The invention provides a high-brightness coating material, which comprises a substrate, an Nb layer and a color layer, wherein the Nb layer is formed on the surface of the substrate, the color layer is formed on the surface of the Nb layer, which is far away from the substrate, the thickness of the Nb layer is 140 nm-500 nm, and the color layer sequentially comprises first SiO in the direction far away from the Nb layer2Film layer, first Nb2O5Film layer, second SiO2Film layer, second Nb2O5A film layer, wherein the first SiO2The thickness of the film layer is 71-77 nm, and the first Nb2O5The thickness of the film layer is 52 to56nm, the second SiO2The thickness of the film layer is 84-90 nm, and the second Nb is2O5The thickness of the film layer is 51-55 nm.
As a preferred embodiment of the present invention, an orange coating material is provided, which includes a substrate, an Nb layer and a color layer, wherein the Nb layer is formed on a surface of the substrate, the color layer is formed on a surface of the Nb layer away from the substrate, a thickness of the Nb layer is 140nm to 500nm, and the color layer sequentially includes a first Nb layer and a second Nb layer along a direction away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 33-37 nm, and the first SiO layer2The thickness of the film layer is 73-79 nm, and the second Nb is2O5The thickness of the film layer is 71-75 nm, and the second SiO is2The thickness of the film layer is 137-143 nm, and the third Nb2O5The thickness of the film layer is 52-56 nm, and the third SiO is2The thickness of the film layer is 137-143 nm, and the fourth Nb is2O5The thickness of the film layer is 74-78 nm, and the fourth SiO is2The thickness of the film layer is 224-230 nm.
As a preferred embodiment of the present invention, a dark blue coating material is provided, which includes a substrate, an Nb layer and a color layer, wherein the Nb layer is formed on a surface of the substrate, the color layer is formed on a surface of the Nb layer facing away from the substrate, a thickness of the Nb layer is 140nm to 500nm, and the color layer sequentially includes a first Nb layer along a direction facing away from the Nb layer2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 49-53 nm, and the first SiO layer2The thickness of the film layer is 93-99 nm, and the second Nb is2O5The thickness of the film layer is 54-58 nm, and the second SiO is2The thickness of the film layer is 63-69 nm, and the third Nb2O5The thickness of the film layer is 19-23 nm, and the third SiO is2The thickness of the film layer is 80-86 nm, and the fourth Nb is2O5The thickness of the film layer is 47-51 nm, and the fourth SiO is2The thickness of the film layer is 110-116 nm.
Another embodiment of the present invention provides a method for preparing the coating material, including the following steps:
placing the substrate under a vacuum condition, bombarding the Nb target by adopting an ion source, depositing and forming an Nb layer on the surface of the substrate, and controlling the thickness of the Nb layer to be more than or equal to 140 nm;
and bombarding a target corresponding to the high-refraction layer and a target corresponding to the low-refraction layer by ions on the basis of the Nb layer and introducing auxiliary gas to form the high-refraction layer and the low-refraction layer which are alternated on the Nb layer.
In a preferred embodiment, an Nb layer, a high refractive layer or a low refractive layer is formed using Ion Beam Assisted Deposition (IBAD), a target made of the metal to be deposited, oxygen or nitrogen implantation being combined with the ion beam bombarded target when required. Therefore, the sputtering process is performed with a metal target, when forming the Nb layer, the Nb target is bombarded by an ion beam to sputter Nb particles from the Nb target, the Nb particles are deposited on the surface of the substrate to form the Nb layer, when forming the high refractive layer or the low refractive layer, the corresponding metal is used as the target, and by using O as the target2Or N2The ion beam strikes the deposited metal to convert the very thin film formed on the substrate to an oxide or nitride. For example, the target for sputtering may be made of pure Nb or Si, while the ion beam includes O containing argon ions2Or N2To form SiO2、Si3N4、Nb2O5And the like.
In some embodiments, before the Nb layer is deposited, argon gas is introduced under vacuum, the ion source is turned on, and the surface of the substrate is subjected to ion cleaning for 2-5 min.
The impurities on the surface of the base material can be effectively removed by carrying out ion cleaning on the surface of the base material, and the bonding strength between the base material and the Nb layer is improved to a certain extent.
The present invention will be further illustrated by the following examples.
Example 1
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes the following steps:
SiO2the film is obtained by sputtering Si target material; elementary substances Nb and Nb2O5Obtained by sputtering Nb target.
a. Placing the aluminum alloy base material on a clamp of a sputtering machine, and vacuumizing;
b. the vacuum degree of the chamber to be coated reaches 3 multiplied by 10-3When Pa, introducing argon, after the gas is stable, opening an ion source, and carrying out ion cleaning on the surface of the substrate for 2-5 min;
c. the ion source continues to work, and meanwhile, a sputtering power supply of the Nb target is started, the power is 10KW, the thickness is 184nm, and the coating of the No. 1 Nb layer is completed;
d. oxygen of an ion source is opened, the flow rate is 200sccm, the Nb target power supply is continuously opened, and Nb is deposited2O5A film layer with the thickness of 27nm is formed, and the 2 nd film coating is finished;
e. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 20nm is formed, and the 3 rd film coating is finished;
f. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 37nm is formed, and the 4 th film coating is finished;
g. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 60nm is formed, and the 5 th film coating is finished;
h. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 100nm is formed, and the 6 th film coating is finished;
i. the sputtering power supply of the Nb target is turned offStarting a Si target power supply, enabling the oxygen flow to be 150sccm, and depositing SiO2A film layer with the thickness of 31nm is formed, and the first final layer of film coating is finished;
j. after the coating is finished, the Si target power supply is turned off, the ion source power supply is turned off, then argon and oxygen are turned off, the rotation of the rotary frame is stopped, after the temperature of the workpiece is reduced, the refrigerator is started to defrost, finally, the air is filled, the temperature is restored to the atmospheric pressure, and the workpiece is taken out, so that the obtained coating material is shown in figure 1.
Example 2
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes most of the operation steps in example 1, and the differences are as follows:
the substrate is selected from glass, and the obtained coating material is shown in figure 2.
Example 3
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes most of the operation steps in example 1, and the differences are as follows:
the substrate is selected from white ceramics, and the obtained coating material is shown in figure 3.
Example 4
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes most of the operation steps in example 1, and the differences are as follows:
the thickness of the Nb layer was 145 nm.
Example 5
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes most of the operation steps in example 1, and the differences are as follows:
the thickness of the Nb layer was 490 nm.
Example 6
The comparative example is used for comparative explanation of the coating material and the preparation method thereof disclosed by the invention, and comprises most of the operation steps of example 1, and the differences are that:
the thickness of the Nb layer was 600 nm.
Example 7
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes the following steps:
SiO2the film is obtained by sputtering Si target material; elementary substances Nb and Nb2O5Obtained by sputtering Nb target.
a. Placing the aluminum alloy base material on a clamp of a sputtering machine, and vacuumizing;
b. the vacuum degree of the chamber to be coated reaches 3 multiplied by 10-3When Pa, introducing argon, after the gas is stable, opening an ion source, and carrying out ion cleaning on the surface of the substrate for 2-5 min;
c. the ion source continues to work, and meanwhile, a sputtering power supply of the Nb target is started, the power is 10KW, the thickness is 184nm, and the coating of the No. 1 Nb layer is completed;
d. the sputtering power supply of the Nb target is closed, the oxygen of the ion source is turned on, the oxygen flow is 150sccm, the Si target power supply is turned on, and SiO is deposited2A film layer with the thickness of 74nm is formed, and the 2 nd film coating is finished;
e. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 54nm is formed, and the 3 rd film coating is completed;
f. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 87nm is formed, and the 4 th film coating is finished;
g. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 53nm is formed, and the final film coating is finished;
h. after the coating is finished, the Nb target power supply is turned off, the ion source power supply is turned off, then argon and oxygen are turned off, the rotation of the rotating frame is stopped, after the workpiece is cooled, the refrigerator is started to defrost, finally, the gas is filled, the atmosphere is recovered, and the workpiece is taken out, so that the coating material is obtained as shown in figure 4.
Example 8
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes the following steps:
SiO2the film is obtained by sputtering Si target material; elementary substances Nb and Nb2O5By sputtering NbAnd (4) obtaining the target material.
a. Placing the aluminum alloy base material on a clamp of a sputtering machine, and vacuumizing;
b. the vacuum degree of the chamber to be coated reaches 3 multiplied by 10-3When Pa, introducing argon, after the gas is stable, opening an ion source, and carrying out ion cleaning on the surface of the substrate for 2-5 min;
c. the ion source continues to work, and meanwhile, a sputtering power supply of the Nb target is started, the power is 10KW, the thickness is 184nm, and the coating of the 1 st covering layer is completed;
d. oxygen of an ion source is opened, the flow rate is 200sccm, the Nb target power supply is continuously opened, and Nb is deposited2O5A film layer with the thickness of 35nm is formed, and the 2 nd film coating is finished;
e. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 76nm is formed, and the 3 rd film coating is finished;
f. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5Coating the film layer with the thickness of 73nm to finish the 4 th coating;
g. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 140nm is formed, and the 5 th film coating is finished;
h. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 54nm is formed, and the 6 th film coating is finished;
i. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 140nm is formed, and the 7 th film coating is finished;
j. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 76nm is formed, and the 8 th film coating is finished;
k. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 227nm is formed, and the 9 th film coating is finished;
and l, after the coating is finished, closing the Si target power supply, closing the ion source power supply, then closing argon and oxygen, stopping the rotation of the rotating frame, starting a refrigerator to defrost after the workpiece is cooled, finally inflating, recovering to atmospheric pressure, and taking out to obtain the coating material as shown in fig. 5.
Example 9
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes the following steps:
SiO2the film is obtained by sputtering Si target material; elementary substances Nb and Nb2O5Obtained by sputtering Nb target.
a. Placing the aluminum alloy base material on a clamp of a sputtering machine, and vacuumizing;
b. when the vacuum degree of the film coating chamber reaches 3 multiplied by 10 < -3 > Pa, introducing argon, after the gas is stable, opening an ion source, and carrying out ion cleaning on the surface of the substrate for 2-5 min;
c. the ion source continues to work, and meanwhile, a sputtering power supply of the Nb target is started, the power is 10KW, the thickness is 184nm, and the coating of the 1 st covering layer is completed;
d. oxygen of an ion source is opened, the flow rate is 200sccm, the Nb target power supply is continuously opened, and Nb is deposited2O5A film layer with the thickness of 51nm is formed, and the 2 nd film coating is finished;
e. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 96nm is formed, and the 3 rd film coating is finished;
f. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 56nm is formed, and the 4 th film coating is finished;
g. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 66nm is formed, and the 5 th film coating is finished;
h. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 21nm is formed, and the 6 th film coating is finished;
i. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, and oxygen flowsMeasuring 150sccm, depositing SiO2A film layer with the thickness of 83nm is formed, and the 7 th film coating is finished;
j. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5Coating a film layer with the thickness of 49nm to finish the 8 th coating;
k. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 113nm is formed, and the 9 th film coating is finished;
and l, after the coating is finished, closing the Si target power supply, closing the ion source power supply, then closing argon and oxygen, stopping the rotation of the rotating frame, starting a refrigerator to defrost after the workpiece is cooled, finally inflating, recovering to atmospheric pressure, and taking out to obtain the coating material as shown in fig. 6.
Example 10
This example is used to illustrate the coating material and the preparation method thereof disclosed by the present invention, and includes the following steps:
SiO2the film is obtained by sputtering Si target material; elementary substances Nb and Nb2O5Obtained by sputtering Nb target.
a. Placing the aluminum alloy base material on a clamp of a sputtering machine, and vacuumizing;
b. the vacuum degree of the chamber to be coated reaches 3 multiplied by 10-3When Pa, introducing argon, after the gas is stable, opening an ion source, and carrying out ion cleaning on the surface of the substrate for 2-5 min;
c. the ion source continues to work, and meanwhile, a sputtering power supply of the Nb target is started, the power is 10KW, the thickness is 184nm, and the coating of the 1 st covering layer is completed;
d. oxygen of an ion source is opened, the flow rate is 200sccm, the Nb target power supply is continuously opened, and Nb is deposited2O5A film layer with the thickness of 36nm is formed, and the 2 nd film coating is finished;
e. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2Coating the film layer with the thickness of 85nm to finish the 3 rd film coating;
f. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 82nm is formed, and the 4 th film coating is finished;
g. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 130nm is formed, and the 5 th film coating is finished;
h. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5Coating the film layer with the thickness of 78nm to finish the 6 th film coating;
i. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 66nm is formed, and the 7 th film coating is finished;
j. and after the film coating is finished, closing the Si target power supply, closing the ion source power supply, then closing argon and oxygen, stopping the rotation of the rotating frame, starting a refrigerator to defrost after the workpiece is cooled, finally inflating, and taking out after the workpiece is recovered to the atmospheric pressure.
Comparative example 1
The comparative example is used for comparing and explaining the coating material and the preparation method thereof disclosed by the invention, and comprises the following operation steps:
SiO2and the simple substance SI is obtained by adopting a sputtering Si target material coating mode; nb2O5Obtained by sputtering Nb target.
a. Placing the aluminum alloy base material on a clamp of a sputtering machine, and vacuumizing;
b. the vacuum degree of the chamber to be coated reaches 3 multiplied by 10-3When Pa, introducing argon, after the gas is stable, opening an ion source, and carrying out ion cleaning on the surface of the substrate for 2-5 min;
c. the ion source continues to work, and simultaneously, a sputtering power supply of the Si target is started, the power is 10KW, the thickness is 184nm, and the coating of the 1 st layer of the Si layer is completed;
d. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 27nm is formed, and the 2 nd film coating is finished;
e. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2Film layer, thickness 20nm, finish No. 3Coating a film;
f. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 37nm is formed, and the 4 th film coating is finished;
g. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 60nm is formed, and the 5 th film coating is finished;
h. the sputtering power supply of the Si target is closed, the Nb target power supply is opened, the oxygen flow is 200sccm, and Nb is deposited2O5A film layer with the thickness of 100nm is formed, and the 6 th film coating is finished;
i. the sputtering power supply of the Nb target is closed, the Si target power supply is opened, the oxygen flow is 150sccm, and SiO is deposited2A film layer with the thickness of 31nm is formed, and the first final layer of film coating is finished;
j. and after the coating is finished, closing the Si target power supply, closing the ion source power supply, then closing argon and oxygen, stopping the rotation of the rotary frame, starting a refrigerator to defrost after the workpiece is cooled, finally inflating, recovering to atmospheric pressure, and taking out to obtain the coating material.
Comparative example 2
The comparative example is used for comparative explanation of the coating material and the preparation method thereof disclosed by the invention, and comprises most of the operation steps of example 1, and the differences are that:
the thickness of the Nb layer was 100 nm.
Performance testing
Firstly, Lab value tests are performed on the coating materials prepared in the above examples 1 to 10, and the obtained results are filled in Table 1.
Performing a spectrum test on the coating materials prepared in the embodiments 1 to 3 and the comparative examples 1 and 2, wherein the reflectivity curve test result obtained in the embodiments 1 to 3 is shown in FIG. 7; the results of the reflectance curve test obtained in comparative example 1 are shown in fig. 8; the results of the reflectance curve test obtained in comparative example 2 are shown in fig. 9.
TABLE 1
Colour values L a b Direct viewing color
Example 1 68.6 -9.7 16.5 Yellow green
Example 2 66.5 -1.7 17.4 Yellow green
Example 3 67.3 -4.1 19.8 Yellow green
Example 4 68.6 -9.6 16.6 Yellow green
Example 5 68.8 -9.8 16.4 Yellow green
Example 6 68.9 -9.9 16.2 Yellow green
Example 7 93.2 -9.1 4.2 High bright color
Example 8 45.5 69.4 53.2 Orange colour
Example 9 22.4 89.2 -109 Deep blue color
Example 10 29.2 55.8 21.2 Red colour
Comparative example 1 57.8 -14.1 5.27 Grass green
Comparative example 2 49.4 -13.8 14.29 Dark green color
As can be seen from the test data of the examples 1 to 5 and the comparative examples 1 and 2 in the table 1, the influence of different base materials on the Lab value of the coating material is small, and the Lab values of the examples are relatively close, which shows that the Nb layer can effectively shield the influence of the base materials on the final color effect of the coating material, and the shielding effect of the Nb layer is directly related to the thickness of the Nb layer, so that the deviation between the actual color parameter and the design parameter of the coating material can be caused when the thickness is too low. From the test data of the embodiments 7 to 10, it can be seen that the coating material prepared by the preparation method provided by the invention has a wider color range by adjusting the thicknesses and the numbers of the high reflection layer and the low reflection layer. As can be seen from fig. 8, after the Nb layer is replaced with the Si layer, the reflectance curve of the plated film layer of comparative example 1 has a significant deviation from the designed curve, which makes it difficult to adjust the film layer to achieve the desired color effect. It can be seen from fig. 9 that the reflection curve of comparative example 2 changes significantly, the corresponding color value also changes significantly, and there is a large difference with example 1, which indicates that the substrate cannot be well shielded after the Nb layer is below a certain thickness, and the material of the substrate itself affects the final formed color.
Secondly, carrying out a hundred-lattice adhesion test on the coating materials prepared in the embodiments 1-10 and the comparative examples 1 and 2, and carrying out a hundred-lattice adhesion test after boiling for half an hour:
and (3) testing the hundred-lattice adhesive force:
(1) before testing, the appearance is checked to be abnormal, no color change, air bubbles, cracks, falling off and the like exist, and the surface of the base material is wiped clean by using dust-free cloth;
(2) holding a cutting tool, wherein a tool face is perpendicular to a test face to prevent a tool edge from tilting a film layer when a cutting grid is cut, the cutting grid direction forms an angle of 45 degrees with a sample, and the cutting tool is uniformly applied with force (the force is that the tool edge just penetrates through the film layer to reach a substrate) to form 10 multiplied by 10 continuous square small grids of 1 multiplied by 1 mm;
(3) brushing fragments of a test area by using dust-free cloth, uniformly pulling out a section of adhesive tape, removing the foremost section, then cutting off the adhesive tape with the length of about 55mm, placing the central point of the adhesive tape above a grid in a direction parallel to a group of cutting lines, and then flattening the part of the adhesive tape above the grid area by using a nail to ensure that the adhesive tape is in good contact with a film layer (the nail is not allowed to scratch the adhesive tape and the film layer), wherein the length of the adhesive tape at least exceeds 20mm of the grid;
(4) sticking an adhesive tape, standing for 90s, holding the suspended end of the adhesive tape, and quickly pulling down the adhesive tape within 0.5-1.0s at an angle as close to 60 degrees as possible;
(5) and (3) checking the film peeling condition, wherein the film peeling condition is qualified when the film peeling condition reaches or exceeds 4B, and the specific evaluation standard is as follows:
5B: the cutting edge is completely smooth without falling off;
4B: a little coating falls off at the intersection of the cuts, and the affected cross cutting area is not more than 5%;
3B: the coating is stripped at the intersection of the cuts and/or along the edges of the cuts, and the affected cross cutting area is more than 5 percent but not more than 15 percent;
2B: the film layer partially or totally falls off in large fragments along the cut edges and/or partially or totally falls off on different parts of the grid, the affected cross cut area is more than 15% but not more than 35%;
1B: the coating is peeled off along large fragments of the cutting edge, and/or some squares are partially or completely peeled off, and the affected cross cutting area is more than 35 percent but not more than 65 percent;
0B: the degree of exfoliation exceeded 1B.
Test results are filled in Table 2
TABLE 2
Figure BDA0002547919230000161
As can be seen from the test results in Table 2, the coating material prepared by the preparation method provided by the invention has high adhesion.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (14)

1. The coating material is characterized by comprising a base material, an Nb layer and a color layer, wherein the Nb layer is formed on the surface of the base material, the color layer is formed on the surface, away from the base material, of the Nb layer, the thickness of the Nb layer is larger than or equal to 140nm, the color layer comprises a plurality of low-refraction layers and a plurality of high-refraction layers, and the low-refraction layers and the high-refraction layers are alternately laminated.
2. The plating material according to claim 1, wherein the thickness of the Nb layer is 140nm to 500 nm.
3. The coating material of claim 1, wherein the substrate comprises one or more of a ceramic, a glass, a metal, and an organic material.
4. The coating material of claim 1, wherein the refractive index of the low-refractive layer is less than 1.75, and the refractive index of the high-refractive layer is greater than 1.9.
5. The plating material according to claim 1, wherein the low-refraction layer comprises SiO2、MgF2、Al2O3One or more of (a).
6.The plating material of claim 1, wherein the high-refraction layer comprises Nb2O5、Si3N4、TiO2、Ti3O5And ZrO.
7. The coating material according to claim 5 or 6, wherein the low refractive layer is selected from SiO2The high refractive layer is selected from Nb2O5。
8. The plating material according to claim 1, wherein the low-refractive layer has a single-layer thickness of 5 to 400nm, and the high-refractive layer has a single-layer thickness of 5 to 400 nm.
9. The coating material of claim 1, wherein the color layers comprise a first Nb in sequence in a direction away from the Nb layers2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 25-29 nm, and the first SiO is2The thickness of the film layer is 17-23 nm, and the second Nb is2O5The thickness of the film layer is 35-39 nm, and the second SiO is2The thickness of the film layer is 57-63 nm, and the third Nb is2O5The thickness of the film layer is 98-102 nm, and the third SiO is2The thickness of the film layer is 28-34 nm.
10. The coating material of claim 1, wherein the color layers comprise a first Nb in sequence in a direction away from the Nb layers2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 34-38 nm, and the first SiO layer2The thickness of the film layer is 82-88 nm, and the second Nb is2O5The thickness of the film layer is 79-84 nm, and the second SiO is2The thickness of the film layer is 127-133 nm, and the third Nb2O5The thickness of the film layer is 76-80 nm, and the third SiO is2The thickness of the film layer is 63-69 nm.
11. The coating material of claim 1, wherein the color layer comprises, in order, a first SiO in a direction away from the Nb layer2Film layer, first Nb2O5Film layer, second SiO2Film layer, second Nb2O5A film layer, wherein the first SiO2The thickness of the film layer is 71-77 nm, and the first Nb2O5The thickness of the film layer is 52-56 nm, and the second SiO is2The thickness of the film layer is 84-90 nm, and the second Nb is2O5The thickness of the film layer is 51-55 nm.
12. The coating material of claim 1, wherein the color layers comprise a first Nb in sequence in a direction away from the Nb layers2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 33-37 nm, and the first SiO layer2The thickness of the film layer is 73-79 nm, and the second Nb is2O5The thickness of the film layer is 71-75 nm, and the second SiO is2The thickness of the film layer is 137-143 nm, and the third Nb2O5The thickness of the film layer is 52-56 nm, and the third SiO is2The thickness of the film layer is 137-143 nm, and the fourth Nb is2O5The thickness of the film layer is 74-78 nm, and the fourth SiO is2The thickness of the film layer is 224-230 nm.
13. The coating material of claim 1, wherein the color layers comprise a first Nb in sequence in a direction away from the Nb layers2O5Film layer, first SiO2Film layer, second Nb2O5Film layer, second SiO2Film layer, third Nb2O5Film layer, third SiO2Film layer, fourth Nb2O5Film layer, fourth SiO2A film layer, wherein the first Nb2O5The thickness of the film layer is 49-53 nm, and the first SiO layer2The thickness of the film layer is 93-99 nm, and the second Nb is2O5The thickness of the film layer is 54-58 nm, and the second SiO is2The thickness of the film layer is 63-69 nm, and the third Nb2O5The thickness of the film layer is 19-23 nm, and the third SiO is2The thickness of the film layer is 80-86 nm, and the fourth Nb is2O5The thickness of the film layer is 47-51 nm, and the fourth SiO is2The thickness of the film layer is 110-116 nm.
14. The method for preparing the coating material according to any one of claims 1 to 13, comprising the following steps:
placing the substrate under a vacuum condition, bombarding the Nb target by adopting an ion source, depositing and forming an Nb layer on the surface of the substrate, and controlling the thickness of the Nb layer to be more than or equal to 140 nm;
and bombarding a target corresponding to the high-refraction layer and a target corresponding to the low-refraction layer by ions on the basis of the Nb layer and introducing auxiliary gas to form the high-refraction layer and the low-refraction layer which are alternated on the Nb layer.
CN202010566202.8A 2020-06-19 2020-06-19 Coating material and preparation method thereof Pending CN113817986A (en)

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