CN112458408A - Method for preparing high-light-reflection multicolor gradient coating composite base material - Google Patents

Method for preparing high-light-reflection multicolor gradient coating composite base material Download PDF

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CN112458408A
CN112458408A CN202011088548.8A CN202011088548A CN112458408A CN 112458408 A CN112458408 A CN 112458408A CN 202011088548 A CN202011088548 A CN 202011088548A CN 112458408 A CN112458408 A CN 112458408A
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base material
steps
composite
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electron beam
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陈胜利
谢祥斌
习锋
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Dongguan Qipin Optics Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24Vacuum evaporation
    • C23C14/28Vacuum evaporation by wave energy or particle radiation
    • C23C14/30Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/083Oxides of refractory metals or yttrium
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/10Glass or silica

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
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  • Mechanical Engineering (AREA)
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Abstract

The invention discloses a method for preparing a high-reflectivity multicolor gradient coated composite substrate, which comprises the following steps of performing electronic evaporation; step two, stacking and plating; step three, oxidizing and isolating; step four, gradually changing the color light; step five, boxing and storing; according to the method for plating the high-reflection multicolor gradient coated composite base material, the multilayer film is plated on the composite base material by adopting an electron beam evaporation plating method at the temperature of 80 ℃, the low expansion coefficient of zirconium oxide is utilized, the better chemical stability is well matched with the base material, the plated film layer is compact, and the possibility of insecurity of the direct contact film layer between the titanium oxide layer and the base material is reduced; the stability of the film layer in a cold and hot impact environment is also ensured due to the characteristic of low expansion coefficient; according to the optical film theory, based on the multi-beam interference effect, the materials with high refractive index and low refractive index are mutually superposed, and the titanium oxide and the silicon oxide realize the high reflection effect of different beams of visible light from red to blue violet, which is opposite to that of the antireflection film.

Description

Method for preparing high-light-reflection multicolor gradient coating composite base material
Technical Field
The invention relates to the technical field of composite substrates, in particular to a method for preparing a high-light-reflection multicolor gradient coated composite substrate.
Background
In the fields of electronic component consumer products, mobile phone appearance decorating parts, clocks, vehicle-mounted screens and the like, because the technical field of current mobile phone application and the development of software technology and hardware technology are limited by certain technological innovation, terminal client developers urgently need to find a novel trend of breaking point energy benches, 5G comes to find and apply composite materials, the traditional composite base material film has poor uniformity and low compactness, and the problems of film cracking and falling caused by stress generated by a thick coating film on the composite base material cannot be solved; aiming at the defects, a method for designing a highly reflective multicolor gradient coated composite substrate is necessary.
Disclosure of Invention
The invention aims to provide a method for preparing a high-reflectivity multicolor gradient coated composite substrate, which aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing a high-reflectivity multicolor gradient coated composite substrate comprises the steps of performing electronic evaporation; step two, stacking and plating; step three, oxidizing and isolating; step four, gradually changing the color light; step five, boxing and storing;
wherein in the first step, the electron evaporation comprises the steps of:
1) manually preparing an electron beam evaporator, and cleaning and disinfecting the evaporator;
2) selecting a proper composite PMMA + PC base material, placing the composite PMMA + PC base material in an electron beam evaporator, and plating a zirconium dioxide isolation layer through the electron beam evaporator;
in the second step, the stack plating comprises the following steps:
1) taking out the composite PMMA + PC base material with the zirconium dioxide isolating layer in the step one 2), standing and cooling, and then putting into an electron beam evaporator again;
2) starting an electron beam evaporator, and plating metal titanium oxide, titanium dioxide or titanium pentoxide and silicon dioxide doped titanium oxide on the isolation layer by electron beam evaporation in sequence;
in the third step, the oxidation isolation comprises the following steps:
1) separating the surface of the prepared resin layer on the composite base material by a zirconia layer, and repeatedly stacking to prepare titanium metal oxide and silicon dioxide;
2) the stacked zirconia layer is 10-20 nm; the controllable range of the thickness of the stacked titanium oxide and silicon oxide is 400-1000nm, so that the high-light-reflection multicolor gradient coating composite substrate can be obtained;
in the fourth step, the color light gradual change comprises the following steps:
1) cleaning the composite PMMA + PC base material processed in the step three 2), drying and standing;
2) placing the film in an atmospheric environment at a natural room temperature, wherein the visible light reflecting layer or the multiple color light reflecting layers formed by the stacking thickness gradually change, and the reflected light can reach 75-80%;
in the fifth step, the high-reflectivity multicolor gradient coating composite base material in the fourth step 2) is manually detected, packaged and stored in a shady and cool place.
According to the technical scheme, the thickness of the isolation layer in the step one 2) is 10-20 nm.
According to the technical scheme, the composite base material to be coated in the step one 2) is cleaned and pretreated by deionized water and dried; heating the substrate to be coated at 80 deg.C to adsorb water vapor molecules, removing by vacuum pump in vacuum environment, and pumping to 3.0-4.5 x 10-3pa。
According to the technical scheme, the design ratio of the total thickness of the titanium pentoxide and the silicon dioxide in the step three 2) is 1: 1; the thickness can be designed to be 400-1000 nm.
According to the technical scheme, in the step four 2), the high-reflectivity can reach that R is 75-80%, and the visible light wavelength presents a range W of 400-650 nm.
Compared with the prior art, the invention has the following beneficial effects: according to the method for plating the high-reflection multicolor gradient coated composite base material, the multilayer film is plated on the composite base material by adopting an electron beam evaporation plating method at the temperature of 80 ℃, the low expansion coefficient of zirconium oxide is utilized, the better chemical stability is well matched with the base material, the plated film layer is compact, and the possibility of insecurity of the direct contact film layer between the titanium oxide layer and the base material is reduced; the stability of the film layer in a cold and hot impact environment is also ensured due to the characteristic of low expansion coefficient; according to the optical film theory, based on the multi-beam interference effect, the materials with high refractive index and low refractive index are mutually superposed, and the titanium oxide and the silicon oxide realize the high reflection effect of different beams of visible light from red to blue violet, which is opposite to that of the antireflection film.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Referring to fig. 1, the present invention provides a technical solution:
example 1:
a method for preparing a high-reflectivity multicolor gradient coated composite substrate comprises the steps of performing electronic evaporation; step two, stacking and plating; step three, oxidizing and isolating; step four, gradually changing the color light; step five, boxing and storing;
wherein in the first step, the electron evaporation comprises the steps of:
1) manually preparing an electron beam evaporator, and cleaning and disinfecting the evaporator;
2) selecting a proper composite PMMA + PC base material, placing the composite PMMA + PC base material in an electron beam evaporator, and passing through the electron beam evaporatorPlating a zirconium dioxide isolation layer, wherein the thickness of the isolation layer is 10-20 nm; cleaning and pretreating the composite base material to be coated with deionized water, and drying; heating the substrate to be coated at 80 deg.C to adsorb water vapor molecules, removing by vacuum pump in vacuum environment, and pumping to 3.0-4.5 x 10-3pa, bulk vacuum 3.0 x 10-3pa, MFC: 10sccm, Maxpower300MA, using compressed cake or column zirconium oxide, without powder film material, to reduce powder impurity and gassing effect, with a deposition thickness of 10 nm;
in the second step, the stack plating comprises the following steps:
1) taking out the composite PMMA + PC base material with the zirconium dioxide isolating layer in the step one 2), standing and cooling, and then putting into an electron beam evaporator again;
2) starting electron beam evaporation machine, plating titanium oxide, titanium oxide and silicon oxide on the isolating layer by electron beam evaporation, and vacuum-pumping the body by 3.0 x 10-3pa, APC: 1.0 x 10-2pa, the silicon oxide rate is 5-7a/s, the plating scheme meets the condition that the evacuation time is more than 25min, the temperature of the cavity in the plated film actually reaches 80 ℃, and titanium dioxide or titanium pentoxide and silicon dioxide doped titanium oxide can be repeatedly stacked in sequence for plating; the silicon oxide column and the powder can be both, the titanium oxide is evaporated by small light spots, the deposition thickness is designed according to the ratio of 1:1, and the plating is carried out according to the required reflectivity and color light. Wherein the refractive index of titanium oxide is 2.25, and the refractive index of silicon oxide is 1.58;
in the third step, the oxidation isolation comprises the following steps:
1) separating the surface of the prepared resin layer on the composite base material by a zirconia layer, and repeatedly stacking to prepare titanium metal oxide and silicon dioxide;
2) the stacked zirconia layer is 10-20 nm; the thickness controllable range of the stacked titanium oxide and silicon oxide is 400-1000nm, and the design ratio of the total thickness of the titanium pentoxide and the silicon dioxide is 1: 1; the thickness can be designed to be 400-1000nm, and the high-light-reflection multicolor gradient coating composite substrate can be obtained;
in the fourth step, the color light gradual change comprises the following steps:
1) cleaning the composite PMMA + PC base material processed in the step three 2), drying and standing;
2) placing the film in an atmospheric environment at a natural room temperature, wherein a visible light reflecting layer or a plurality of color light reflecting layers formed by stacking thickness gradually change, the reflected light can reach 75-80%, the high reflection can reach 75-80%, the visible light wavelength presentation range W is 400-650nm, the obtained film is continuously processed for 96h by using a QUV instrument and comprises 12 cycles of 8h, the film is subjected to single-cycle UV irradiation UV-a of 4h, 340nm, 0.63W/M2, 3M600 drawing OK at 60 ℃, the conventional monomer test meets the requirements, the film thickness on the surface of the film-coated composite substrate under a D65 light source is 400nm, the surface of the film is compact and has no chap, and the film-coated substrate is subjected to boiling water at 100 ℃ and has no shedding after being boiled for 60 min;
in the fifth step, the high-reflectivity multicolor gradient coating composite base material in the fourth step 2) is manually detected, packaged and stored in a shady and cool place.
Example 2:
a method for preparing a high-reflectivity multicolor gradient coated composite substrate comprises the steps of performing electronic evaporation; step two, stacking and plating; step three, oxidizing and isolating; step four, gradually changing the color light; step five, boxing and storing;
wherein in the first step, the electron evaporation comprises the steps of:
1) manually preparing an electron beam evaporator, and cleaning and disinfecting the evaporator;
2) selecting a proper composite PMMA + PC base material, placing the composite PMMA + PC base material in an electron beam evaporator, and plating a zirconium dioxide isolation layer through the electron beam evaporator, wherein the thickness of the isolation layer is 10-20 nm; cleaning and pretreating the composite base material to be coated with deionized water, and drying; heating the substrate to be coated at 80 deg.C to adsorb water vapor molecules, removing by vacuum pump in vacuum environment, and pumping to 3.0-4.5 x 10-3pa, plating isolation layer, vacuum 4.5 x 10 of bulk- 3pa, MFC: 15sccm, Maxpower200MA, using compressed cake or column zirconium oxide, without powder film material, to reduce powder impurity and gassing effect, with a deposition thickness of 20 nm;
in the second step, the stack plating comprises the following steps:
1) taking out the composite PMMA + PC base material with the zirconium dioxide isolating layer in the step one 2), standing and cooling, and then putting into an electron beam evaporator again;
2) starting electron beam evaporation machine, plating titanium oxide, titanium oxide and silicon oxide on the isolating layer by electron beam evaporation, and vacuum-pumping the body 4.5 x 10-3pa,APC:1.0*10-2pa, the silicon oxide rate is 5-7a/s, the plating scheme meets the requirement that the evacuation time is more than 25min, the temperature of the cavity in the plated film actually reaches 80 ℃, both silicon oxide cylinders and powder can be used, titanium oxide is evaporated in small light spots, the deposition thickness is designed according to the ratio of 1:1, the refractive index of titanium oxide is 2.25, the refractive index of silicon oxide is 1.58, the plating process does not adopt plasma Ar positive charge ion deposition, the surface of the composite substrate is subjected to ionization surface treatment before the isolation layer is plated, the surface energy is reduced, the dust ion adsorption force and organic matter treatment on the surface of substances under a microstructure are removed, and titanium dioxide or titanium pentoxide and silicon dioxide doped titanium oxide can be repeatedly stacked in sequence for plating;
in the third step, the oxidation isolation comprises the following steps:
1) separating the surface of the prepared resin layer on the composite base material by a zirconia layer, and repeatedly stacking to prepare titanium metal oxide and silicon dioxide;
2) the stacked zirconia layer is 10-20 nm; the thickness controllable range of the stacked titanium oxide and silicon oxide is 400-1000nm, and the design ratio of the total thickness of the titanium pentoxide and the silicon dioxide is 1: 1; the thickness can be designed to be 400-1000nm, and the high-light-reflection multicolor gradient coating composite substrate can be obtained;
in the fourth step, the color light gradual change comprises the following steps:
1) cleaning the composite PMMA + PC base material processed in the step three 2), drying and standing;
2) placing the film in an atmospheric environment at a natural room temperature, wherein a visible light reflecting layer or a plurality of color light reflecting layers formed by stacking thickness gradually change, the reflected light can reach 75-80%, the high reflection can reach 75-80%, the visible light wavelength presentation range W is 400-650nm, the obtained film is continuously processed for 96h by using a QUV instrument and comprises 12 cycles of 8h, the film is subjected to single-cycle UV irradiation UV-a of 4h, 340nm, 0.63W/M2 and 3M600 drawing OK at 60 ℃, the conventional monomer test meets the requirements, the film thickness on the surface of the film-coated composite substrate under a D65 light source is 1000nm, the surface of the film is compact and has no chap, and the film-coated substrate is subjected to boiling water at 100 ℃ and has no shedding after being boiled for 60 min;
in the fifth step, the high-reflectivity multicolor gradient coating composite base material in the fourth step 2) is manually detected, packaged and stored in a shady and cool place.
The properties of the examples are compared in the following table:
62-68 Dain pen test Reflectivity of light Rule of gradual change
Example 1 The surface of the substrate satisfies 76% Order of
Example 2 The surface of the substrate satisfies 78% Order of
Based on the above, the method for preparing the high-reflection multicolor gradient coated composite base material has the advantages that the method adopts an electron beam evaporation coating method at 80 ℃ at high temperature to coat the multilayer film on the composite base material, the low expansion coefficient of zirconium oxide is utilized, the better chemical stability is well matched with the base material, the coated film layer is compact, and the possibility of insecurity of the direct contact film layer between the titanium oxide layer and the base material is reduced; the stability of the film layer in a cold and hot impact environment is also ensured due to the characteristic of low expansion coefficient; according to the optical film theory, based on the multi-beam interference effect, the materials with high refractive index and low refractive index are mutually superposed, and the titanium oxide and the silicon oxide realize the high reflection effect of different beams of visible light from red to blue violet, which is opposite to that of the antireflection film.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A method for preparing a high-reflectivity multicolor gradient coated composite substrate comprises the steps of performing electronic evaporation; step two, stacking and plating; step three, oxidizing and isolating; step four, gradually changing the color light; step five, boxing and storing; the method is characterized in that:
wherein in the first step, the electron evaporation comprises the steps of:
1) manually preparing an electron beam evaporator, and cleaning and disinfecting the evaporator;
2) selecting a proper composite PMMA + PC base material, placing the composite PMMA + PC base material in an electron beam evaporator, and plating a zirconium dioxide isolation layer through the electron beam evaporator;
in the second step, the stack plating comprises the following steps:
1) taking out the composite PMMA + PC base material with the zirconium dioxide isolating layer in the step one 2), standing and cooling, and then putting into an electron beam evaporator again;
2) starting an electron beam evaporator, and plating metal titanium oxide, titanium dioxide or titanium pentoxide and silicon dioxide doped titanium oxide on the isolation layer by electron beam evaporation in sequence;
in the third step, the oxidation isolation comprises the following steps:
1) separating the surface of the prepared resin layer on the composite base material by a zirconia layer, and repeatedly stacking to prepare titanium metal oxide and silicon dioxide;
2) the stacked zirconia layer is 10-20 nm; the controllable range of the thickness of the stacked titanium oxide and silicon oxide is 400-1000nm, so that the high-light-reflection multicolor gradient coating composite substrate can be obtained;
in the fourth step, the color light gradual change comprises the following steps:
1) cleaning the composite PMMA + PC base material processed in the step three 2), drying and standing;
2) placing the film in an atmospheric environment at a natural room temperature, wherein the visible light reflecting layer or the multiple color light reflecting layers formed by the stacking thickness gradually change, and the reflected light can reach 75-80%;
in the fifth step, the high-reflectivity multicolor gradient coating composite base material in the fourth step 2) is manually detected, packaged and stored in a shady and cool place.
2. The method for preparing a highly reflective multicolor gradient coated composite substrate according to claim 1, wherein the method comprises the following steps: the thickness of the isolation layer in the step one 2) is 10-20 nm.
3. The method for preparing a highly reflective multicolor gradient coated composite substrate according to claim 1, wherein the method comprises the following steps: cleaning and pretreating the composite base material to be coated in the step one 2) by using deionized water, and drying; heating the substrate to be coated at 80 deg.C to adsorb water vapor molecules, removing by vacuum pump in vacuum environment, and pumping to 3.0-4.5 x 10-3pa。
4. The method for preparing a highly reflective multicolor gradient coated composite substrate according to claim 1, wherein the method comprises the following steps: the design ratio of the total thickness of the titanium pentoxide and the silicon dioxide in the step three 2) is 1: 1; the thickness can be designed to be 400-1000 nm.
5. The method for preparing a highly reflective multicolor gradient coated composite substrate according to claim 1, wherein the method comprises the following steps: in the step four 2), the high reflectivity can reach 75-80%, and the visible light wavelength presents in the range W of 400-650 nm.
CN202011088548.8A 2020-10-13 2020-10-13 Method for preparing high-light-reflection multicolor gradient coating composite base material Pending CN112458408A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109023280A (en) * 2018-09-17 2018-12-18 深圳市三海科技有限公司 A kind of method that magnetron sputter prepares graduated colors film

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109023280A (en) * 2018-09-17 2018-12-18 深圳市三海科技有限公司 A kind of method that magnetron sputter prepares graduated colors film

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Application publication date: 20210309