WO2024093106A1 - 一种清底色防蓝光防红外树脂镜片及其制备方法 - Google Patents

一种清底色防蓝光防红外树脂镜片及其制备方法 Download PDF

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WO2024093106A1
WO2024093106A1 PCT/CN2023/084292 CN2023084292W WO2024093106A1 WO 2024093106 A1 WO2024093106 A1 WO 2024093106A1 CN 2023084292 W CN2023084292 W CN 2023084292W WO 2024093106 A1 WO2024093106 A1 WO 2024093106A1
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layer
resin lens
infrared
composite oxide
proof
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PCT/CN2023/084292
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English (en)
French (fr)
Inventor
黄昱勇
汤峰
吴仲英
董光平
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江苏万新光学有限公司
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Publication of WO2024093106A1 publication Critical patent/WO2024093106A1/zh

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    • G—PHYSICS
    • G02—OPTICS
    • G02C—SPECTACLES; SUNGLASSES OR GOGGLES INSOFAR AS THEY HAVE THE SAME FEATURES AS SPECTACLES; CONTACT LENSES
    • G02C7/00—Optical parts
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/086—Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • 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
    • C23C14/12—Organic material
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/28—Vacuum evaporation by wave energy or particle radiation
    • C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
    • 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
    • G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
    • G02B1/041—Lenses
    • 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
    • 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
    • G02B1/14—Protective coatings, e.g. hard coatings
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/28—Interference filters
    • G02B5/281—Interference filters designed for the infrared light
    • G02B5/282—Interference filters designed for the infrared light reflecting for infrared and transparent for visible light, e.g. heat reflectors, laser protection
    • 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

Definitions

  • the present invention relates to the technical field of resin lens preparation, and in particular to a clear-bottom-color, blue-light-proof, infrared-proof, and high-temperature-resistant resin lens and a preparation method thereof.
  • a film is generally coated on the surface of the resin lens to reduce the reflection of light and enhance the transmission of light, which is an optical anti-reflection film.
  • Near-infrared is not sensitive to the human eye and is mainly absorbed by the cornea, which has potential damage to the human eye.
  • the optical film layer has the characteristics of anti-reflection and infrared protection.
  • Such an optical film layer is much thicker than a general conventional film layer.
  • the main material of the optical film is an inorganic material, and the polymer resin lens substrate is an organic material, the difference in the physical and chemical properties of the two leads to higher stress in the lens after coating, which in turn leads to poor temperature resistance and durability.
  • the film layer with a clear background color and infrared protection function is generally thicker, and its effect on the stress of the lens after coating is particularly significant, which affects its normal use. Therefore, how to provide a low-reflection, infrared-proof, high-temperature-resistant and durable resin lens has become an urgent problem to be solved in this field.
  • Blue light protection can effectively protect consumers from the demands of electronic use environments.
  • the new national blue light protection standard also distinguishes between harmful blue light and beneficial blue light.
  • blue light protection usually makes the lenses more yellow and less bright.
  • the present invention aims to provide a clear background color, blue light protection, infrared protection and high temperature resistant resin lens and a preparation method thereof, which can effectively meet the anti-reflection requirements, achieve good infrared protection effect, improve the high temperature resistance and durability of the resin lens by reducing stress, and use special processes to plate special materials to meet the national blue light protection standards and clear background color visual effects.
  • the first aspect of the present invention provides a clear base color, blue light proof, infrared proof and high temperature resistant resin lens, comprising: a resin lens substrate, a hardened layer and a clear base color infrared proof layer; wherein the resin lens substrate, the hardened layer and the clear base color infrared proof film layer are arranged in sequence, the hardened layer is located on the surface of the resin lens substrate, and the clear base color infrared proof film layer is located on the surface of the hardened layer;
  • the UV cut-off wavelength of the resin lens substrate is 405-407nm;
  • the clear base color infrared-proof and high temperature-resistant resin lens further comprises a waterproof layer, and the waterproof layer is located on the surface of the clear base color infrared-proof film layer;
  • the material of the hardened layer is organic silicon; further preferably, the organic silicon contains at least Ti element;
  • the clear background color anti-infrared film layer includes a silicon-aluminum composite oxide layer, a titanium-niobium composite oxide layer, a tin-doped indium oxide (i.e., ITO) layer, and a titanium nitride (TiN) layer; further, the clear background color anti-infrared film layer includes three layers of silicon-aluminum composite oxide layers, three layers of titanium-niobium composite oxide layers, a layer of tin-doped indium oxide (i.e., ITO) layer, a layer of silicon dioxide, and a layer of titanium nitride (TiN);
  • the silicon-aluminum composite oxide layer is composed of a composite material of SiO 2 and Al 2 O 3 , wherein the molar fraction of SiO 2 in the composite material is 70% to 95%; further preferably, wherein the molar fraction of SiO 2 in the composite material is 92%;
  • the titanium-niobium composite oxide layer is composed of a composite material of TiO 2 and Nb 2 O 5 , wherein TiO 2 accounts for 10% to 90% of the molar fraction of the composite material; preferably, wherein TiO 2 accounts for 80% of the molar fraction of the composite material;
  • the purity of TiN in the titanium nitride layer is greater than 99.9%;
  • the thickness of the hardened layer is 1 to 5 ⁇ m
  • the thickness of the clear base color anti-infrared film layer is 290 to 950 nm;
  • the thickness of the waterproof layer is 4 to 20 nm
  • the average reflectivity of the clear-base-color blue-light-proof and infrared-proof resin high-temperature-resistant lens is ⁇ 1.5%;
  • the near infrared blocking rate of the clear base color anti-blue light and anti-infrared resin high temperature resistant lens is greater than 55%
  • the yellow index of the clear base color anti-blue light and anti-infrared resin high temperature resistant lens is ⁇ 4.5%
  • the second aspect of the present invention provides a method for preparing the above-mentioned clear base color blue light and infrared resistant resin high temperature resistant lens, comprising the following steps:
  • S1 preparing a hard layer: forming a hard layer on the surface of a resin lens substrate, that is, obtaining a resin lens containing a hard layer;
  • S2 preparing a clear background color infrared-proof film layer: forming the clear background color infrared-proof film layer on the surface of the resin lens obtained in S1, that is, obtaining a resin lens containing a clear background color infrared-proof film layer, specifically comprising:
  • step S23 forming a fourth SiO2- containing resin lens on the surface of the resin lens obtained in step S22;
  • step S24 forming a fifth titanium-niobium composite oxide layer, a sixth silicon-aluminum composite oxide layer, and a seventh titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S23;
  • step S25 forming an eighth ITO-containing resin lens on the surface of the resin lens obtained in step S24;
  • step S3 preparing a waterproof layer: forming a waterproof layer on the surface of the resin lens obtained in step S2.
  • the present invention adopts a specific UV405 resin lens substrate to make the lens close to the blue light protection standard and maintain a low yellow index;
  • the present invention adopts a specific film layer to make the lens have the effects of infrared protection, blue light protection and clear background color, which specifically includes: (1)
  • the film layer is prepared by using titanium niobium composite oxide material to have infrared protection effect, improve the temperature resistance and durability of the product, and improve the repeatability and mass production of the product, and significantly improve the temperature resistance and durability of the lens: a.
  • TiO2 doped with a certain molar ratio of Nb2O5 can effectively avoid the easy crystallization characteristics of the TiO2 film layer, and can also effectively avoid the defect of the dense Nb2O5 film layer being easy to crack on the resin lens.
  • the film layer Under the condition of low ion source energy for coating the resin glasses, the film layer is ensured to be in an amorphous state to prevent the film layer from cracking due to crystallization, thereby improving the high temperature and high humidity resistance of the film layer and the lens, and further improving the durability of the product; b.
  • the film layer material is doped with TiO2 and Nb2O5 , the influence of TiO2 on O in the IAD auxiliary process is reduced. 2.
  • the sensitivity of the flow rate is reduced, the process difficulty is reduced and the repeatability and mass production of the product are effectively improved: c.
  • the film material adopts a composite material of TiO 2 and Nb 2 O 5 , and the optical refractive index is close to TiO 2 , which is higher than the refractive index of materials such as Nb 2 O 5 , so that the anti-infrared cutoff effect is better, the reflectivity of the anti-reflection film is lower, and the infrared cutoff is deeper than other existing products, and the light transmittance of the resin lens is improved, so that the lens prepared by the present invention has a good visual effect while protecting the human eye and reducing near-infrared radiation;
  • the TiN layer prepared by a specific process can supplement the anti-blue light standard, enhance infrared blocking, and reduce the yellow index to increase the effect of clearing the background color.
  • the film layer produces 2% absorption on one side of the 415-445nm band, which is important for the anti-blue light standard, to ensure that the lens meets the anti-blue light standard and protect the human eye from blue light damage; the absorption of yellow light is about 0.6% higher than that of blue light, thereby effectively reducing the yellow index and ensuring that the lens is clear and white; the absorption of near-infrared is above 3%, which effectively increases the infrared blocking rate and reduces the damage of infrared to the human eye;
  • the present invention uses a silicon-aluminum composite oxide layer and a SiO2 layer in combination, which effectively avoids the formation of long columns by SiO2, resulting in high stress in the film layer, maintains the glassy structure of the film layer, and improves the high temperature resistance of the film layer.
  • Fig. 1 is a schematic diagram of the layers of a clear base color infrared-proof resin lens prepared in Examples 1 to 4 of the present invention; a resin lens substrate 1, a hardened layer 2, a clear base color infrared-proof film layer 3, and a waterproof layer 4; wherein the clear base color infrared-proof film layer 3 includes: a silicon-aluminum composite oxide layer 3-1, a titanium-niobium composite oxide layer 3-2, a titanium nitride layer 3-3 plated by a special process, a silicon dioxide layer 3-4, a titanium-niobium composite oxide layer 3-5, a silicon-aluminum composite oxide layer 3-6, a titanium-niobium composite oxide layer 3-7, an ITO layer 3-8, and a silicon-aluminum composite oxide layer 3-9
  • the clear background color infrared protection film layer includes three silicon aluminum composite oxide layers, three titanium niobium composite oxide layers, a titanium nitride layer, a silicon dioxide layer and a tin-doped indium oxide (i.e., ITO) layer, wherein the clear background color infrared protection film layer includes the following layers in order: (1) silicon aluminum composite oxide layer, (2) titanium niobium composite oxide layer, (3) titanium nitride layer, (4) silicon dioxide layer, (5) titanium niobium composite oxide layer, (6) silicon aluminum composite oxide layer, (7) titanium niobium composite oxide layer, (8) tin-doped indium oxide (i.e., ITO) layer, and (9) silicon aluminum composite oxide layer; and the first silicon aluminum composite oxide layer is located on the surface of the hardened layer;
  • each layer of the clear base color anti-infrared film layer is:
  • the thickness of the first silicon-aluminum composite oxide layer is 0 to 180 nm, preferably 5 to 30 nm;
  • the thickness of the second titanium-niobium composite oxide layer is 10 to 40 nm, preferably 10 to 20 nm;
  • the thickness of the third titanium nitride layer is 0.5 to 2 nm, preferably 0.7 to 1.2 nm;
  • the thickness of the fourth silicon dioxide layer is 20 to 60 nm, preferably 30 to 50 nm;
  • the thickness of the fifth titanium-niobium composite oxide layer is 80 to 150 nm, preferably 100 to 120 nm;
  • the thickness of the sixth silicon-aluminum composite oxide layer is 90 to 250 nm, preferably 140 to 200 nm;
  • the thickness of the seventh titanium-niobium composite oxide layer is 80 to 150 nm, preferably 90 to 110 nm;
  • the thickness of the eighth ITO layer is 2 to 10 nm, preferably 5 nm;
  • the thickness of the ninth silicon-aluminum composite oxide layer is 60 to 130 nm, preferably 65 to 90 nm;
  • the step of preparing the hardened layer in S1 comprises: immersing the ultrasonically cleaned resin lens substrate into a 25-30% by weight hardening solution aqueous solution at a dipping temperature of 10-20° C., dipping for 4-8 seconds and then pulling out the solution at a speed of 1.0-3.0 mm/s, and then drying it at 70-90° C. for 2-5 hours, then taking out the substrate and sending it to a drying oven for drying and curing, the curing temperature is 100-150° C., and the curing time is 120-180 min, to obtain a resin lens containing a hardened layer;
  • the process of preparing the clear base color infrared protection film layer in step S2 comprises:
  • a vacuum coating process is adopted to evaporate silicon-aluminum composite oxide layer, titanium-niobium composite oxide, titanium nitride, silicon dioxide and ITO solid film layer materials, and then transmit them through the gas phase to deposit them into a thin film on the surface of the resin lens obtained in step S1 to form a clear base color anti-infrared film layer, which specifically includes the following steps:
  • step S21 forming a first layer of silicon-aluminum composite oxide on the surface of the resin lens obtained in step S1, heating the silicon-aluminum composite oxide with a high-energy electron beam at a rate of 1000 ⁇ under the conditions of a background vacuum of ⁇ 3 ⁇ 10 -3 Pa, a temperature in the coating chamber of 50-70°C, and an ion source-assisted process. Depositing the evaporated silicon-aluminum composite oxide in the form of nano-scale molecules to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
  • step S22 forming a titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S21, heating the titanium-niobium composite oxide on the surface of the resin lens obtained in step S21 by using a high-energy electron beam at a rate of depositing the evaporated titanium-niobium composite oxide in the form of nano-scale molecules to obtain a resin lens containing a second titanium-niobium composite oxide layer;
  • step S23 forming a titanium nitride layer on the surface of the resin lens obtained in step S22, specifically comprising:
  • S231 first evacuate to a background vacuum degree of ⁇ 8 ⁇ 10 -4 Pa, then bombard with an ion source Hall source for 50 to 80 seconds, the ion source bombardment parameters are: anode voltage: 90 to 140 V, anode current: 2.5 to 5 A, auxiliary gas is Ar, and the flow rate is 5 to 20 sccm; preferably, the ion source Hall source bombardment time is 60 seconds, and the ion source bombardment parameters are: anode voltage: 110 V, anode current: 3 A, auxiliary gas is Ar, and the flow rate is 10 sccm;
  • S232 Deposition in an ion source assisted process, using a high energy electron beam to heat TiN at a rate
  • the evaporated TiN is deposited in the form of nano-scale molecules.
  • the auxiliary parameters of the ion source are: anode voltage: 90-140V, anode current: 2.5-5A, auxiliary gas is Ar and N2 , Ar flow rate is 5-15sccm, N2 flow rate is: 3-15sccm; preferably, under the assistance of the ion source, at a rate
  • the evaporated TiN is deposited in the form of nano-scale molecules
  • the auxiliary parameters of the ion source are: anode voltage: 110V, anode current: 3A, auxiliary gas is Ar and N2 , Ar flow rate is 10sccm, N2 flow rate is: 5sccm;
  • the bombardment parameters are: anode voltage: 90 to 140 V, anode current: 2.5 to 5 A, auxiliary gas is Ar and N 2 , Ar flow rate is 5 to 15 sccm, N 2 flow rate is 3 to 15 sccm; preferably, the bombardment time is 30 seconds, the bombardment parameters are: anode voltage: 110 V, anode current: 3 A, auxiliary gas is Ar and N 2 , Ar flow rate is 10 sccm, N 2 flow rate is 5 sccm;
  • the evaporated SiO2 is deposited in the form of nano-scale molecules to obtain a resin lens containing a SiO2 layer;
  • the ion source auxiliary parameters are: anode voltage: 90-140V, anode current: 2.5-5A, auxiliary gas is Ar, and the flow rate is 5-20sccm; preferably, the ion source is assisted at a rate of
  • the evaporated SiO 2 was deposited in the form of nano-scale molecules, and the ion source bombardment auxiliary parameters were: anode voltage: 110 V, anode current: 3 A, auxiliary gas was Ar, and the flow rate was 10 sccm;
  • step S25 repeating step S22 to form a titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S24;
  • step S26 repeat step S21 to form a silicon-aluminum composite oxide layer on the surface of the resin lens obtained in step S25;
  • step S27 repeat step S22 to form a titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S26;
  • the ion source assisted deposition process parameters are: the ion source is a Hall source, the anode voltage is 90 to 140 V, the anode current is 2.5 to 5 A, the auxiliary gas is O 2 , and the flow rate is 10 to 30 sccm; preferably, the ion source assisted deposition process parameters are: the ion source is a Hall source, the anode voltage is 110 V, the anode current is 3 A, the auxiliary gas is O 2 , and the flow rate is 15 sccm;
  • the step S3: forming a waterproof layer on the surface of the resin lens obtained in step S2 comprises the following steps: continuing to use a vacuum coating process on the surface of the lens obtained in step S29, using a high-energy electron beam to heat the material at a rate of 1000 °C under the conditions that the background vacuum degree is ⁇ 3 ⁇ 10 -3 Pa and the temperature in the coating chamber is 50-70°C.
  • Depositing the evaporated fluorine-containing waterproof material preferably a waterproof material containing perfluoroalkane (C 12 F 27 N)
  • C 12 F 27 N perfluoroalkane
  • the titanium nitride material has a molecular formula of TiN and a purity of 99.9%, and is made by sintering titanium nitride powder using a conventional process, and is specifically commissioned to Changzhou Zhanchi Optoelectronics Technology Co., Ltd. for development and production;
  • the silicon-aluminum composite oxide is developed and produced by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the silicon-aluminum composite oxide layer is composed of a composite material of SiO 2 and Al 2 O 3 , and the molar fraction of SiO 2 in the composite material is 70% to 95%.
  • the embodiments and comparative examples please refer to the embodiments and comparative examples;
  • the titanium-niobium composite oxide is developed and produced by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the titanium-niobium composite oxide is composed of TiO 2 and Nb 2 O 5 , wherein the molar fraction of TiO 2 is 10% to 90%.
  • specific models please refer to the examples and comparative examples;
  • the resin lens substrate selected in the present invention is a conventional lens in the art, and the content of the UV powder is adjusted so that the UV cut-off wavelength is 405-407 nm.
  • the definition of the UV cut-off wavelength refers to 5.4.2.4.4 of the optical resin lens standard QB/T 2506-2017;
  • a resin lens substrate with model MR-8 (refractive index 1.60) or MR-7 (refractive index 1.67) and a UV cutoff wavelength of 405 to 407 nm is purchased from Mitsui Chemicals, Inc. of Japan, hereinafter referred to as "MR-8-UV405" or "MR-7-UV405"; or in a specific embodiment, a resin lens substrate with a refractive index of 1.56 and a UV cutoff wavelength of 405 to 407 nm developed and produced by Jiangsu Shike New Materials Co., Ltd. is purchased, hereinafter referred to as "SK1.56-UV405".
  • SK1.56-UV405" for the specific preparation method of the resin lens substrate, refer to the patent of Shike Optics Co., Ltd.: CN201410245692.6.
  • the present invention can select a conventional hardening liquid.
  • a conventional hardening liquid for example, in a specific embodiment, the hardening liquid model Z117 or Z118 (hereinafter referred to as "Z117” or “Z118") of Ito Optical Industry Co., Ltd. is selected; or in a specific embodiment, the hardening liquid model VH56 (hereinafter referred to as "VH56”) of Dun Optics (Changshu) Co., Ltd. is selected. Selecting the hardening liquid for coating greatly improves the dense connection between the film layers.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/12.48nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/1.0nm, silicon dioxide layer 3-4/34.5nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.5nm, silicon aluminum composite oxide layer 3-101.66/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.6nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/71.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm);
  • the method for preparing the resin lens comprises the following steps:
  • step S2 preparing a clear background color infrared-proof film layer: in a vacuum coating machine, using a vacuum coating process, evaporating the solid film layer material and then transmitting it through the gas phase, and depositing it into a thin film on the surface of the resin lens obtained in step S1 to form a clear background color infrared-proof film layer, specifically comprising the following steps:
  • step S21 forming a silicon-aluminum composite oxide layer on the surface of the resin lens obtained in step S1.
  • a background vacuum of ⁇ 3 ⁇ 10 -3 Pa
  • a high-energy electron beam is used to heat the silicon-aluminum composite oxide at a rate of Depositing the evaporated silicon-aluminum composite oxide in the form of nano-scale molecules to obtain a resin lens containing a first silicon-aluminum composite oxide layer;
  • step S22 Forming a titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S21.
  • a high-energy electron beam is used to heat the titanium-niobium composite oxide at a rate of depositing the evaporated titanium-niobium composite oxide in the form of nano-scale molecules to obtain a resin lens containing a second titanium-niobium composite oxide layer;
  • S23 forming a titanium nitride layer on the surface of the resin lens obtained in step S22, specifically comprising the following steps: S231: first evacuating to a background vacuum of ⁇ 8 ⁇ 10 -4 Pa, and then bombarding with an ion source Hall source for 60 seconds, the ion source bombardment parameters are: anode voltage: 110V, anode current: 3A, auxiliary gas is Ar, flow rate is 10sccm; S232: depositing under the ion source assisted process, using a high-energy electron beam to heat TiN at a rate The evaporated TiN is deposited in the form of nano-scale molecules, and the auxiliary parameters of the ion source are: anode voltage: 110V, anode current: 3A, auxiliary gases are Ar and N2 , Ar flow rate is 10sccm, N2 flow rate is: 5sccm; S233: continue to bombard the TiN film layer surface with the ion source Hall source for 30 seconds, and the bombardment parameters are: an
  • S24 The surface of the resin lens obtained in S23 is heated by a high-energy electron beam at a rate of 10000 t/ cm2 , with a background vacuum of ⁇ 3 ⁇ 10 -3 Pa, a temperature in the coating chamber of 50-70°C, and an ion source assisted process.
  • the evaporated SiO 2 is deposited in the form of nano-scale molecules to obtain a resin lens containing a SiO 2 layer;
  • the auxiliary parameters of the ion source are: anode voltage: 110V, anode current: 3A, auxiliary gas is Ar, and the flow rate is 10sccm.
  • step S25 repeating step S22 to form a titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S24;
  • step S26 repeat step S21 to form a silicon-aluminum composite oxide layer on the surface of the resin lens obtained in step S25;
  • step S27 Repeat step S22 to form a titanium-niobium composite oxide layer on the surface of the resin lens obtained in step S26;
  • step S3 preparing a waterproof layer: forming a waterproof layer on the surface of the resin lens obtained in step S29: continuing to use a vacuum coating process on the surface of the lens obtained in step S29, using a high-energy electron beam to heat the material at a rate of 1000 °C under the conditions that the background vacuum degree is ⁇ 3 ⁇ 10 -3 Pa and the temperature in the coating chamber is 60°C.
  • the evaporated waterproof material containing C 12 F 27 N is deposited in the form of nano-scale molecules on the surface of the resin lens obtained in S24 to obtain the lens.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (SK1.56-UV405); a hardening layer 2 (VH56)/1-2.6 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/11.8nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/1.0nm, silicon dioxide layer 3-4/35.26nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.2nm, silicon aluminum composite oxide layer 3-6/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.7nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/70.83nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm).
  • the method for preparing the resin lens comprises the following steps:
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-7-UV405); a hardening layer 2 (Z118)/1-2.6 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/14.34nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/1.0nm, silicon dioxide layer 3-4/34.1nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/116.05nm, silicon aluminum composite oxide layer 3-6/160.78nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.34nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/70.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm).
  • the method for preparing the resin lens comprises the following steps:
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/12.48nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/0.75nm, silicon dioxide layer 3-4/34.5nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.5nm, silicon aluminum composite oxide layer 3-6/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.6nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/71.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm);
  • the preparation method is the same as that of Example 1.
  • a clear bottom color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardened layer 2 (Z117)/2.6-3 ⁇ m; a light green infrared-proof film layer 3 comprising: a SiO2 layer 3-1/24.6 nm, a ZrO2 layer 3-2/8.42 nm, a SiO2 layer 3-3/51.42 nm, a ZrO2 layer 3-4/118.72 nm, a SiO2 layer 3-5/160.59 nm, a ZrO2 layer 3-6/80.64 nm , an ITO layer 3-7/5 nm; a SiO2 layer 3-8/66.3 nm; a waterproof layer 4 (adopting a waterproof material containing C12F27N / 10 nm);
  • the preparation method comprises the following steps:
  • step S2 preparing a clear background color infrared-proof film layer: in a vacuum coating machine, using a vacuum coating process, evaporating the solid film layer material and then transmitting it through the gas phase, and depositing it into a thin film on the surface of the resin lens obtained in step S1 to form a clear background color infrared-proof film layer, specifically comprising the following steps:
  • the surface of the resin lens obtained in S1 is heated by high-energy electron beam at a rate of 10000 t/ cm2 , with a background vacuum of ⁇ 3 ⁇ 10 -3 Pa, a temperature of 60°C in the coating chamber, and no ion source auxiliary process.
  • the evaporated SiO 2 is deposited in the form of nano-scale molecules to obtain a resin lens containing a first SiO 2 layer;
  • S212 The surface of the resin lens obtained in S211 is heated by high-energy electron beam at a rate of 1000 ⁇ to 2000 ⁇ under the conditions of background vacuum ⁇ 3 ⁇ 10 -3 Pa, temperature in the coating chamber of 60°C, and no ion source auxiliary process.
  • the evaporated ZrO 2 is deposited in the form of nano-scale molecules to obtain a resin lens containing a second ZrO 2 layer;
  • S213 repeating steps S211 and S212 to alternately form a third SiO 2 layer, a fourth ZrO 2 layer, a fifth SiO 2 layer, and a sixth ZrO 2 layer, respectively, to form a resin lens including a third SiO 2 layer, a fourth ZrO 2 layer, a fifth SiO 2 layer, and a sixth ZrO 2 layer;
  • S3 preparing a waterproof layer: forming a waterproof layer on the surface of the resin lens obtained in S23: continuing to use the vacuum coating process on the surface of the lens obtained in step S2, using a high-energy electron beam to heat the material at a rate of 1000 °C under the conditions that the background vacuum degree is ⁇ 3 ⁇ 10 -3 Pa and the temperature in the coating chamber is 60°C.
  • the evaporated waterproof material containing C 12 F 27 N is deposited in the form of nano-scale molecules on the surface of the resin lens obtained in S24 to obtain the lens.
  • a blue anti-reflection and infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8- UV405 ); a hardening layer 2 (Z117)/2.6-3 ⁇ m; an anti-reflection layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO2 and Al2O3 is: 92% SiO2 : 8% Al2O3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/27.6nm, a titanium- niobium composite oxide layer 3-2 (wherein the molar percentage of TiO2 and Nb2O5 is : 80 % TiO2 : 20% Nb2O5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/15.45nm, silicon-aluminum composite oxide layer 3-3/31.42nm (material is the same as 3-1), titanium-niobium composite oxide layer 3-4 (material is the same as 3-2)/98.9nm, silicon-aluminum composite oxide layer 3-5/171.92nm (material is the same as 3-1), titanium - niobium composite oxide layer 3-6 (material is the same as 3-2)/91.96nm, ITO layer 3-7/5nm; silicon-aluminum composite oxide layer 3-8/75.8nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C12F27N /10nm);
  • the method for preparing the resin lens comprises the following steps:
  • step S2 Preparation of anti-reflection and infrared protection layer:
  • a vacuum coating process is adopted to evaporate the solid film material and then transmit it through the gas phase, and then deposit it into a thin film on the surface of the resin lens obtained in step S1 to form an anti-reflection and infrared protection layer, which specifically includes the following steps:
  • S212 The surface of the resin lens obtained in S211 is heated by a high-energy electron beam at a rate of 1000 ⁇ under the conditions of a background vacuum of ⁇ 3 ⁇ 10 -3 Pa, a temperature in the coating chamber of 60°C, and an ion source-assisted process. depositing the evaporated titanium-niobium composite oxide in the form of nano-scale molecules to obtain a resin lens containing a second titanium-niobium composite oxide layer;
  • S213 repeating steps S211 and S212 to alternately form a third silicon-aluminum composite oxide layer, a fourth titanium-niobium composite oxide layer, a fifth silicon-aluminum composite oxide layer, and a sixth titanium-niobium composite oxide layer, respectively, that is, forming a resin lens including a third silicon-aluminum composite oxide layer, a fourth titanium-niobium composite oxide layer, a fifth silicon-aluminum composite oxide layer, and a sixth titanium-niobium composite oxide layer;
  • S3 preparing a waterproof layer: forming a waterproof layer on the surface of the resin lens obtained in S23: continuing to use the vacuum coating process on the surface of the lens obtained in step S2, using a high-energy electron beam to heat the material at a rate of 1000 °C under the conditions that the background vacuum degree is ⁇ 3 ⁇ 10 -3 Pa and the temperature in the coating chamber is 60°C.
  • the evaporated waterproof material containing C 12 F 27 N is deposited in the form of nano-scale molecules on the surface of the resin lens obtained in S24 to obtain the lens.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; an anti-reflection layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/13.48nm, silicon-aluminum composite oxide layer 3-3/34.5nm (material is the same as 3-1), titanium-niobium composite oxide layer 3-4 (material is the same as 3-2)/114.5nm, silicon-aluminum composite oxide layer 3-5/160.4nm (material is the same as 3-1), titanium - niobium composite oxide layer 3-6 (material is the same as 3-2)/101.62nm, ITO layer 3-7/5nm; silicon-aluminum composite oxide layer 3-8/73nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C12F27N /10nm);
  • a clear bottom color infrared-proof resin lens comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; an anti-reflection layer 3 comprising: a SiO2 layer 3-1/26.6 nm, a TiO2 layer 3-2/13.35 nm, a SiO2 layer 3-3/34.8 nm, a TiO2 layer 3-4/113.81 nm, a SiO2 layer 3-5/161.65 nm, a TiO2 layer 3-6/101.11 nm, an ITO layer 3-7/5 nm; a SiO2 layer 3-8/73.6 nm; a waterproof layer 4 (using a waterproof material containing C12F27N /10 nm ); a preparation method thereof comprises the following steps:
  • step S2 preparing a clear background color infrared-proof film layer: in a vacuum coating machine, using a vacuum coating process, evaporating the solid film layer material and then transmitting it through the gas phase, and depositing it into a thin film on the surface of the resin lens obtained in step S1 to form a clear background color infrared-proof film layer, specifically comprising the following steps:
  • the surface of the resin lens obtained in S1 is heated by high-energy electron beam at a rate of 10000 t/ cm2 , with a background vacuum of ⁇ 3 ⁇ 10 -3 Pa, a temperature of 60°C in the coating chamber, and an ion source assisted process.
  • the evaporated SiO 2 is deposited in the form of nano-scale molecules to obtain a resin lens containing a first SiO 2 layer;
  • S212 The surface of the resin lens obtained in S211 is heated by a high-energy electron beam at a rate of 10000 t/ cm2 , with a background vacuum of ⁇ 3 ⁇ 10 -3 Pa, a temperature in the coating chamber of 60°C, and an ion source assisted process. Depositing the evaporated TiO 2 in the form of nano-scale molecules to obtain a resin lens containing a second TiO 2 layer;
  • S213 repeating steps S211 and S212 to alternately form a third SiO 2 layer, a fourth TiO 2 layer, a fifth SiO 2 layer, and a sixth TiO 2 layer, respectively, to form a resin lens including a third SiO 2 layer, a fourth TiO 2 layer, a fifth SiO 2 layer, and a sixth TiO 2 layer;
  • S3 preparing a waterproof layer: forming a waterproof layer on the surface of the resin lens obtained in S23: continuing to use the vacuum coating process on the surface of the lens obtained in step S2, using a high-energy electron beam to heat the material at a rate of 1000 °C under the conditions that the background vacuum degree is ⁇ 3 ⁇ 10 -3 Pa and the temperature in the coating chamber is 60°C.
  • the evaporated waterproof material containing C 12 F 27 N is deposited in the form of nano-scale molecules on the surface of the resin lens obtained in S24 to obtain the lens.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/12.48nm, SiO-Cr absorption layer 3-3 (SiO:Cr molar ratio is 1:1, sintered by Danyang Keda Coating Materials Co., Ltd.)/1.2nm, silicon dioxide layer 3-4/34.5nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.5nm, silicon aluminum composite oxide layer 3-6/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.6nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/71.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm);
  • the preparation method thereof is the same as that of Example 1 except for the 3-3 SiO-Cr absorption layer.
  • the preparation process of the SiO-Cr absorption layer is as follows: a SiO-Cr layer is formed on the surface of the resin lens obtained in step S22. First, the vacuum is evacuated to a background vacuum degree of ⁇ 1.2 ⁇ 10 -4 Pa. Then, the SiO-Cr is deposited under the ion source Hall source assisted process, and a high-energy electron beam is used to heat the SiO-Cr at a rate of The evaporated SiO-Cr is deposited in the form of nano-scale molecules to obtain a resin lens containing a SiO-Cr layer.
  • the auxiliary parameters of the ion source here are: anode voltage: 110V, anode current: 3A, and Ar flow rate of 12sccm.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/12.48nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/1.0nm, silicon dioxide layer 3-4/34.5nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.5nm, silicon aluminum composite oxide layer 3-6/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.6nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/71.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm);
  • the preparation method thereof is the same as that of Example 1 except for the 3-3 layers of titanium nitride.
  • the preparation process of titanium nitride is as follows: a titanium nitride layer is formed on the surface of the resin lens obtained in step S22. First, evacuate to a background vacuum of ⁇ 8 ⁇ 10 -4 Pa. Then bombard with an ion source Hall source for 60 seconds. The ion source bombardment parameters are: anode voltage: 110V, anode current: 3A, auxiliary gas is Ar, and the flow rate is 10sccm. Then, deposit under the ion source Hall source assisted process, use a high-energy electron beam to heat TiN at a rate The evaporated TiN is deposited in the form of nano-scale molecules to obtain a resin lens containing a TiN layer.
  • the ion source auxiliary parameters here are: anode voltage: 110V, anode current: 3A, Ar flow rate is 12sccm, and there is no nitrogen flow rate.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/12.48nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/1.0nm, silicon dioxide layer 3-4/34.5nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.5nm, silicon aluminum composite oxide layer 3-6/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.6nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/71.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm);
  • the preparation method is the same as that of Example 1 except for the 3-3 layer of titanium nitride.
  • the preparation process of titanium nitride is as follows: S23: Form a titanium nitride layer on the surface of the resin lens obtained in step S22. First, evacuate to a background vacuum of ⁇ 8 ⁇ 10 -4 Pa. No ion source Hall source pre-bombardment. Directly deposit under the ion source Hall source assisted process, use a high energy electron beam to heat TiN at a rate The evaporated TiN is deposited in the form of nano-scale molecules to obtain a resin lens containing a TiN layer.
  • the ion source auxiliary parameters here are: anode voltage: 110V, anode current: 3A, Ar flow rate is 10sccm, and nitrogen flow rate is: 5sccm.
  • a clear base color infrared-proof resin lens which comprises, in order: a resin lens substrate 1 (MR-8-UV405); a hardening layer 2 (Z117)/2.6-3 ⁇ m; a clear base color infrared-proof film layer 3 comprising: a silicon-aluminum composite oxide layer 3-1 (wherein the molar percentage of SiO 2 and Al 2 O 3 is: 92% SiO 2 : 8% Al 2 O 3 ; commissioned by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is SA56)/26 nm, a titanium-niobium composite oxide layer 3-2 (wherein the molar percentage of TiO 2 and Nb 2 O 5 is: 80% TiO 2 : 20% Nb 2 O 5 ; Entrusted to Changzhou Zhanchi Optoelectronics Technology Co., Ltd.
  • the material model is PTN28)/12.48nm, titanium nitride layer 3-3 (molecular formula TiN, purity above 99.9%, sintered by Changzhou Zhanchi Optoelectronics Technology Co., Ltd.)/1.0nm, silicon dioxide layer 3-4/34.5nm (molecular formula SiO 2 , purity 99.99%, sintered by Danyang Keda Coating Materials Co., Ltd.), titanium niobium composite oxide layer 3-5 (material is the same as 3-2)/114.5nm, silicon aluminum composite oxide layer 3-6/160.4nm (material is the same as 3-1); titanium niobium composite oxide layer 3-7 (material is the same as 3-2)/101.6nm; ITO layer 3-8/5nm; silicon aluminum composite oxide layer 3-9/71.0nm (material is the same as 3-1); waterproof layer 4 (using waterproof material containing C 12 F 27 N/10nm);
  • the preparation method thereof is the same as that of Example 1 except for the 3-3 layers of titanium nitride.
  • the preparation process of titanium nitride is S23: forming a titanium nitride layer on the surface of the resin lens obtained in step S22.
  • the ion source bombardment parameters are: anode voltage: 110V, anode current: 3A, auxiliary gas is Ar, and the flow rate is 10sccm.
  • deposit under the ion source Hall source assisted process use a high-energy electron beam to heat TiN at a rate of The evaporated TiN is deposited in the form of nano-scale molecules to obtain a resin lens containing a TiN layer.
  • the ion source auxiliary parameters are: anode voltage: 110V, anode current: 3A, Ar flow rate: 10sccm, nitrogen flow rate: 5sccm.
  • the list of materials for the main embodiments and comparative examples is as follows: the one containing TiN or SiO-Cr is a 9-layer anti-infrared film structure, and the one not containing TiN or SiO-Cr is an 8-layer anti-infrared film system.
  • the average reflectivity refers to the visual average reflectivity under C light (a light source with a color temperature of 6774K defined in CIE) illumination, here refers to the reflectivity of a single side
  • the average transmittance refers to the visual average transmittance under C light (a light source with a color temperature of 6774K defined in CIE) illumination, here refers to the transmittance of the same film system coated on both sides
  • the yellow index refers to the yellow index of the lens calculated with reference to QB-T-2506-2001 after coating on both sides
  • the near-infrared transmittance near-infrared average transmittance: here refers to the near-infrared cutoff rate of the lens calculated with reference to QB-T-2506-2017 after coating on both sides
  • the general process uses SiO-Cr as the absorption layer, which can effectively meet the needs of blue light protection. However, its yellow-green light absorption is low, which will lead to an increase in the yellow index. Most weak absorption materials have this characteristic.
  • the use of the specific process of the present invention to prepare the TiN layer can effectively increase the blocking absorption of near-infrared, control the absorption of blue light, and increase the absorption of yellow light, thereby reducing the yellow index and making the lens clearer and more beautiful.
  • Example 1 to 4 and Comparative Examples 1 to 8 After the samples (Examples 1 to 4 and Comparative Examples 1 to 8) were completed, the heat resistance of the samples was tested after being stored for one week.
  • the test method for heat resistance is based on Article 5.8 of the National Heat Resistance Standard for Resin Lenses (GB10810.4-2012): Pass the 55°C 30-minute baking test. After passing the test, the same method is used to increase the temperature by 5°C for 30 minutes each time until the lens shows failure phenomena such as film cracks or orange peel, and the highest qualified temperature is recorded. The results are recorded in Table 5 below.
  • Adhesion test refers to the film adhesion test in accordance with Article 5.9 of the national standard GB10810.4-2012.
  • High-temperature film adhesion test refers to Wanxin Company referring to Article 5.9 of the national standard GB10810.4-2012, changing the boiling conditions to 90 ⁇ 2°C for 60 minutes, and other test methods are the same.
  • Adhesion and high-temperature adhesion test results Grade A refers to no film removal or the film removal area is less than 5%, Grade B refers to the film removal area between 5% and 15%, and Grade C (unqualified) refers to the film removal area significantly greater than 15%.
  • high-temperature adhesion tests were performed from 5 different positions in the coating room. The test results of Examples 1 to 4 and Comparative Examples 1 to 8 are recorded in Table 5 below.
  • the photovoltaic industry and the optical communication industry use high temperature and high humidity to evaluate the durability of products.
  • the high temperature and high humidity test and debugging of the resin lens is defined as: storage at 85°C and 85% humidity for 12 hours, and checking whether the prepared lens has obvious failure phenomena such as film cracks or orange peel; 3 resin lenses are placed in different positions for each high temperature and high humidity test.
  • the test results of Examples 1 to 4 and Comparative Examples 1 to 8 are recorded in Table 5 below.
  • the high-refractive index material of the lens made of titanium-niobium composite oxide has better high-temperature resistance, high-temperature adhesion and durability than other conventional materials
  • the low-refractive index material made of silicon-aluminum composite oxide has better high-temperature resistance, high-temperature adhesion and durability than other conventional materials

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Abstract

本发明提供了一种清底色防蓝光防红外耐高温树脂镜片及其制备方法，包括：树脂镜片基片、加硬层、清底色防红外膜层以及防水层；其中，所述基片、加硬层以及清底色防红外膜层依次排列，所述加硬层位于树脂镜片基片表面，所述清底色防红外膜层位于所述加硬层表面；且所述清底色防红外膜层由高折射率材料钛铌复合氧化物以及低折射率材料硅铝复合氧化物和吸收材料氮化钛组成。本发明通过调整清底色防红外膜层结构以及专门的氮化钛镀制工艺，在满足减反射和防蓝光的同时，获得了具有良好视觉效果的防红外镜片并且极大地提高了树脂镜片耐高温性能和抗环境性能，具有良好市场应用前景。

Description

一种清底色防蓝光防红外树脂镜片及其制备方法 技术领域
本发明涉及树脂镜片制备技术领域，具体涉及一种清底色防蓝光防红外耐高温树脂镜片及其制备方法。
 背景技术
近年来，光学树脂镜片在国内外眼镜市场上需求越来越大，树脂镜片与玻璃镜片相比，具有质量轻、染色性能好、易于加工等优点，中高折射率光学树脂镜片更以高透光率、防紫外、超薄等特有的优势获得使用者的青睐。
为满足树脂镜片光学性能的要求，一般会在树脂镜片表面镀膜，以减少光的反射并增强光的透射，即为光学减反射膜。近红外是人眼不能感光的，主要被角膜吸收，对人眼有着潜在伤害。这要求光学膜层上具备减反射和防红外的特点，这样的光学膜层比一般的常规膜层厚得多。另外，由于光学薄膜的主要材料为无机材料，而高分子树脂镜片基底为有机材料，故因二者物化性质的差异，而导致镀膜后的镜片应力较高，进而导致耐温和耐久性能不佳，尤其是具备清底色防红外功能的膜层一般较厚，其对镀膜后的镜片的应力影响特别显著，而影响其的正常使用。因此，如何提供一种低反射防红外耐高温耐久的树脂镜片成为本领域亟待解决的问题。
防蓝光能够有效防护消费者在电子使用环境中的要求。新的防蓝光国家标准也区分对待有害蓝光和有益蓝光。但是防蓝光通常会造成镜片更黄，不够镁光。为满足消费者在新的电子环境下的新要求，亟需我们提供一种清底色的防蓝光的树脂镜片。
因此需要我们提供综合满足了减反射、防蓝光、防红外等性能和防护要求和清底色的美观要求的新型树脂镜片产品。
发明内容
为克服现有技术缺陷，本发明旨在于提供一种清底色防蓝光防红外耐高温的树脂镜片及其制备方法，有效满足减反射要求，实现良好的防红外效果，通过降低应力来提升树脂镜片的耐高温性和耐久性，并通过专门工艺镀制专门材料来满足国家防蓝光标准和清底色视觉效果。
本发明是通过以下技术方案实现的：
本发明的第一方面提供了一种清底色防蓝光防红外耐高温的树脂镜片，包括：树脂镜片基片、加硬层以及清底色防红外层；其中，所述树脂镜片基片、加硬层以及清底色防红外膜层依次排列，所述加硬层位于所述树脂镜片基片表面，所述清底色防红外膜层位于所述加硬层表面；
所述树脂镜片基片UV截止波长为405～407nm；
进一步的，所述清底色防红外耐高温的树脂镜片还包括防水层，所述防水层位于所述清底色防红外膜层表面；
进一步的，所述加硬层的材料为有机硅；进一步优选的，所述有机硅中至少含有Ti元素；
进一步的，所述清底色防红外膜层包括硅铝复合氧化物层、钛铌复合氧化物层、掺锡氧化铟(即ITO)层以及氮化钛(TiN)层；更进一步的，所述清底色防红外膜层包括三层硅铝复合氧化物层、三层钛铌复合氧化物层、一层掺锡氧化铟(即ITO)层、一层二氧化硅层以及一层氮化钛(TiN)；
进一步的，所述硅铝复合氧化物层由SiO2和Al2O3复合材料组成，且其中SiO2占所述复合材料的摩尔分数为70％～95％；进一步优选的，其中SiO2占所述复合材料摩尔分数的92％；
进一步的，所述钛铌复合氧化物层由TiO2和Nb2O5复合材料组成，其中TiO2占所述复合材料摩尔分数的10％～90％；优选的，其中TiO2占所述复合材料摩尔分数的80％；
进一步的，所述氮化钛层中TiN纯度大于纯度99.9％；
进一步的，所述加硬层的厚度为1～5μm；
进一步的，所述清底色防红外膜层的厚度为290～950nm；
进一步的，所述防水层的厚度为4～20nm；
更进一步的，所述清底色防蓝光防红外树脂耐高温镜片的平均反射率≤1.5％；
更进一步的，所述清底色防蓝光防红外树脂耐高温镜片的近红外阻隔率＞55％；
更进一步的，所述清底色防蓝光防红外树脂耐高温镜片的黄色指数≤4.5％；
本发明第二方面提供了一种上述清底色防蓝光防红外树脂耐高温镜片的制备方法，包括以下步骤：
S1制备加硬层：在树脂镜片基片表面形成加硬层，即获得含加硬层的树脂镜片；
S2制备清底色防红外膜层：在S1获得的树脂镜片表面形成所述清底色防红外膜层，即获得含清底色防红外膜层的树脂镜片，具体包括：
S21：在步骤S1获得的树脂镜片表面分别形成含第一层硅铝复合氧化物层、第二层钛铌复合氧化物层的树脂镜片；
S22：在步骤S21获得的树脂镜片表面形成第三层含氮化钛层的树脂镜片；
S23：在步骤S22获得的树脂镜片表面形成第四层含SiO2层的树脂镜片；
S24：在步骤S23获得的树脂镜片表面形成分别形成第五层钛铌复合氧化物层、第六层硅铝复合氧化物层以及第七层钛铌复合氧化物层的树脂镜片；
S25：在步骤S24获得的树脂镜片表面形成含形成第八层含ITO层的树脂镜片；
S26：在步骤S25获得的树脂镜片表面再形成第九层含硅铝复合氧化物层的树脂镜片；
S3制备防水层：在步骤S2获得的树脂镜片表面形成防水层。
 有益效果
1.本发明采用特定的UV405树脂镜片基片，使镜片接近防蓝光标准，并保持低的黄色指数；
2.本发明采用特定的膜层使得所述镜片具备防红外、防蓝光以及清底色效果，具体包括：(1)采用钛铌复合氧化物材料制备膜层使其具有防红外效果、提升产品耐温性耐久性的同时改善了产品的重复性和可量产性，显著提升了镜片的耐温性和耐久性：a.TiO2掺入一定摩尔比例Nb2O5可以有效规避TiO2膜层的易结晶的特性，也可以有效规避致密的Nb2O5膜层在树脂镜片上易裂的缺陷，在树脂眼镜镀膜低离子源能量的情况下，保证膜层处于无定形态，防止膜层因为结晶崩裂，从而提升膜层和镜片的耐高温和耐高湿性能，进而提高产品的耐久性；b.另外，在制备低反射钛铌复合氧化物膜层时，由于膜层材料由TiO2和Nb2O5掺杂，降低了TiO2对于IAD辅助工艺中O2流量的敏感性，降低了工艺难度并有效改善产品的重复性和可量产性：c.膜层材料采用TiO2和Nb2O5复合材料，并使光学折射率接近TiO2，比Nb2O5等材料的折射率更高，使防红外截止效果更好，减反射膜的反射率较低，比现有的其他产品红外截止更深，并得到提升树脂镜片光透射性，使得本发明制备的镜片，在保护人眼降低近红外辐射的同时具有良好的视觉效果；
(2)采用特定工艺制备的TiN层有补充满足防蓝光标准、增强红外阻隔、降低黄色指数以增加清底色效果，该膜层对防蓝光标准重要的415～445nm波段单面产生了2％的吸收，确保镜片符合防蓝光标准，保护人眼少受蓝光伤害；对黄光的吸收比蓝光高0.6％左右，从而有效降低了黄色指数，保证镜片清澈显白；对近红外的吸收在3％以上，有效的提高了红外阻隔率，降低红外线对人眼的伤害；
(3)提升产品的耐高温性能：本发明采用硅铝复合氧化物层和SiO2层结合使用，有效避免了SiO2容易形成长柱状结果导致膜层高应力，保持膜层的玻璃态结构，提高膜层的耐高温性能。
 附图说明
图1是本发明实施例1～4制备的一种清底色防红外树脂镜片各层示意图；树脂镜片基片1、加硬层2、清底色防红外膜层3、防水层4；其中，清底色防红外膜层3包括：硅铝复合氧化物层3-1、钛铌复合氧化物层3-2、专门工艺镀制的氮化钛层3-3、二氧化硅层3-4、钛铌复合氧化物层3-5、硅铝复合氧化物层3-6、钛铌复合氧化物层3-7、ITO层3-8以及硅铝复合氧化物层3-9
 具体实施方式
在具体实施方式中，所述清底色防红外膜层包括三层硅铝复合氧化物层、三层钛铌复合氧化物层、一层氮化钛层、一层二氧化硅层以及一层掺锡氧化铟(即ITO)层，其中，所述清底色防红外膜层中，所述各层依次为：(1)硅铝复合氧化物层、(2)钛铌复合氧化物层、(3)氮化钛层，(4)二氧化硅层、(5)钛铌复合氧化物层、(6)硅铝复合氧化物层、(7)钛铌复合氧化物层、(8)掺锡氧化铟(即ITO)层、(9)硅铝复合氧化物层；且所述第一层硅铝复合氧化物层位于所述加硬层表面；
更进一步的，在一个具体的实施方式中，所述清底色防红外膜层各层厚度为：
所述第一层硅铝复合氧化物层的厚度为0～180nm，优选5～30nm；
所述第二层钛铌复合氧化物层的厚度为10～40nm，优选10～20nm；
所述第三层氮化钛层的厚度为0.5～2nm，优选0.7～1.2nm；
所述第四层二氧化硅层的厚度为20～60nm，优选30～50nm；
所述第五层钛铌复合氧化物层的厚度为80～150nm，优选100～120nm；
所述第六层硅铝复合氧化物层的厚度为90～250nm，优选140～200nm；
所述第七层钛铌复合氧化物层的厚度为80～150nm，优选90～110nm；
所述第八层ITO层的厚度为2～10nm，优选5nm；
所述第九层硅铝复合氧化物层的厚度为60～130nm，优选65～90nm；
在一个具体的实施方式中，所述S1制备加硬层的步骤包括:将超声波清洗干净的树脂镜片基片浸入质量百分含量25～30％的加硬液水溶液中，浸渍温度10～20℃，浸渍4～8秒后以1.0～3.0mm/s的速度提拉出溶液，再将其于70～90℃烘干2～5小时后将上述基片取出并送至烘干箱内干燥固化，固化温度100～150℃，固化时间120～180min，即得含加硬层的树脂镜片；
在一个具体的实施方式中，所述步骤S2制备清底色防红外膜层的工艺包括：
在真空镀膜机内、采用真空镀膜工艺，将硅铝复合氧化物层、钛铌复合氧化物、氮化钛、二氧化硅以及ITO固态膜层材料蒸发后经过气相传输，在S1步骤获得的树脂镜片表面沉积成薄膜，形成清底色防红外膜层，具体包括以下步骤：
S21：在步骤S1获得的树脂镜片表面形成第一层硅铝复合氧化物层，在本底真空度≤3×10-3Pa、且镀膜舱内温度为50～70℃、有离子源辅助工艺的条件下，采用高能电子束加热所述硅铝复合氧化物，以速率为将蒸发后的硅铝复合氧化物以纳米级分子形式沉积，获得含第一层硅铝复合氧化物层的树脂镜片；
S22：在步骤S21获得的树脂镜片表面形成钛铌复合氧化物层，在S21获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、有离子源辅助工艺的条件下，采用高能电子束加热所述钛铌复合氧化物，以速率为将蒸发后的钛铌复合氧化物以纳米级分子形式沉积，获得含第二层钛铌复合氧化物层的树脂镜片；
S23：在步骤S22获得的树脂镜片表面形成氮化钛层，具体包括：
S231：先抽真空至本底真空度≤8×10-4Pa，再用离子源霍尔源轰击50～80秒，离子源轰击参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar，流量为5～20sccm；优选的，所述离子源霍尔源轰击时间为60秒，离子源轰击参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar，流量为10sccm；
S232：在离子源辅助工艺下沉积，采用高能电子束加热TiN，以速率将蒸发的TiN以纳米级分子形式沉积，所述离子源辅助参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar和N2，Ar流量为5～15sccm、N2流量为：3～15sccm；优选的，在离子源辅助下，以速率将蒸发的TiN以纳米级分子形式沉积，所述离子源辅助参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar和N2，Ar流量为10sccm、N2流量为：5sccm；
S233：继续用离子源霍尔源轰击TiN膜层表面20～40秒，所述轰击参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar和N2，Ar流量为5～15sccm、N2流量为：3～15sccm；优选的，所述轰击时间为30秒，所述轰击参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar和N2，Ar流量为10sccm、N2流量为：5sccm；
S24：在S23获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、并有离子源辅助工艺的条件下，采用高能电子束加热SiO2，以速率为将蒸发后的SiO2以纳米级分子形式沉积，获得含SiO2层的树脂镜片；离子源辅助参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar，流量为5～20sccm；优选的，在离子源辅助下以速率将蒸发的SiO2以纳米级分子形式沉积，离子源轰击辅助参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar，流量为10sccm；
S25：重复S22步骤，在步骤S24获得的树脂镜片表面形成钛铌复合氧化物层；
S26：重复S21步骤，在步骤S25获得的树脂镜片表面形成硅铝复合氧化物层；
S27：重复S22步骤，在步骤S26获得的树脂镜片表面形成钛铌复合氧化物层；
S28：在S27获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、并有离子源辅助工艺的条件下，采用高能电子束加热ITO，以速率为将蒸发后的ITO以纳米级分子形式沉积，获得含ITO层的树脂镜片；
S29：在S28获得的树脂镜片表面，继续采用真空镀膜工艺，重复S21的工艺步骤，再形成一层含硅铝复合氧化物层的树脂镜片；
在S21、S22、S25～S29步骤中，所述离子源辅助沉积工艺参数为：离子源为霍尔源，阳极电压：90～140V，阳极电流：2.5～5A，辅助气为O2，流量为10～30sccm；优选的，所述离子源辅助沉积工艺参数为：离子源为霍尔源，阳极电压：110V，阳极电流：3A，辅助气为O2，流量为15sccm；
在一个具体的实施方式中，所述步骤S3：在S2获得的树脂镜片表面形成防水层包括以下步骤：在S29步骤获得的镜片表面，继续采用真空镀膜工艺，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃条件下，采用高能电子束加热材料，以速率为将蒸发后的含氟防水材料(优选含有全氟烷(C12F27N)的防水材料)以纳米级分子形式进行沉积，获得含防水层的树脂镜片；
在一个具体的实施方式中，所述氮化钛材料，其分子式为TiN，纯度为99.9％，由氮化钛粉末采用常规工艺烧结制成，具体委托常州市瞻驰光电科技股份有限公司开发并生产；
在一个具体的实施方式中，所述硅铝复合氧化物我们委托常州市瞻驰光电科技股份有限公司开发并生产，所述硅铝复合氧化物层由SiO2和Al2O3复合材料组成，且其中SiO2占所述复合材料的摩尔分数为70％～95％，具体型号参见实施例和对比例；
在一个具体的实施方式中，所述钛铌复合氧化物我们委托常州市瞻驰光电科技股份有限公司开发并生产，钛铌复合氧化物由TiO2和Nb2O5组成，其中TiO2的摩尔分数为10％～90％，具体型号参见实施例和对比例；
本发明选择的树脂镜片基片为本领域常规镜片调整其UV粉的含量以UV截止波长在405～407nm即可，UV截止波长的定义参照光学树脂镜片标准QB/T 2506-2017的5.4.2.4.4；
例如，一个具体的实施方式中，购买日本三井化学株式会社的型号为MR-8(折射率1.60)或者MR-7(折射率1.67)、且其UV截止波长为405～407nm的树脂镜片基片，以下简称“MR-8-UV405”或“MR-7-UV405”；或者在一个具体的实施方式中，购买江苏视科新材料股份有限公司开发并生产的折射率为1.56、其UV值截止波长为405～407nm的树脂镜片基片，以下简称“SK1.56-UV405”，该树脂镜片基片具体制备方法参见视客光学公司的专利：CN201410245692.6。
本发明选择常规加硬液体即可，例如在一个具体的实施方式中，选取伊藤光学工业株式会社的型号Z117或Z118(以下简称为“Z117”或“Z118”)加硬液；或者在一个具体的实施方式中选取度恩光学(常熟)有限公司型号为VH56(以下简称为“VH56”)的加硬液，选择加硬液进行镀膜，极大地提高了膜层之间的致密衔接性。
(一)实施例
实施例1
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/12.48nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/1.0nm，二氧化硅层3-4/34.5nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.5nm、硅铝复合氧化物层3-101.66/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.6nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/71.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)；
所述树脂镜片的制备方法包括以下步骤：
S1：制作加硬层：将超声波清洗干净的树脂镜片基片浸入质量百分含量27％、型号为Z117的加硬液水溶液中，浸渍温度15℃，浸渍5秒后以2.0mm/s的速度提拉出溶液；80℃烘干3小时后将上述基片取出并送至烘干箱内干燥固化，固化温度120℃，固化时间150min，即得含加硬层的树脂镜片；
S2制备清底色防红外膜层：在真空镀膜机内、采用真空镀膜工艺，将固态膜层材料蒸发后经过气相传输，在S1步骤获得的树脂镜片表面沉积成薄膜，形成清底色防红外膜层，具体包括以下步骤：
S21：在步骤S1获得的树脂镜片表面形成硅铝复合氧化物层。在本底真空度≤3×10-3Pa、且镀膜舱内温度为50～70℃、有离子源辅助工艺的条件下，采用高能电子束加热所述硅铝复合氧化物，以速率为将蒸发后的硅铝复合氧化物以纳米级分子形式沉积，获得含第一层硅铝复合氧化物层的树脂镜片；
S22：在步骤S21获得的树脂镜片表面形成钛铌复合氧化物层。在S21获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、有离子源辅助工艺的条件下，采用高能电子束加热所述钛铌复合氧化物，以速率为将蒸发后的钛铌复合氧化物以纳米级分子形式沉积，获得含第二层钛铌复合氧化物层的树脂镜片；
S23：在步骤S22获得的树脂镜片表面形成氮化钛层，具体包括以下步骤：S231：先抽真空至本底真空度≤8×10-4Pa，再用离子源霍尔源轰击60秒，离子源轰击参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar，流量为10sccm；S232：在离子源辅助工艺下沉积，采用高能电子束加热TiN，以速率将蒸发的TiN以纳米级分子形式沉积，所述离子源辅助参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar和N2，Ar流量为10sccm、N2流量为：5sccm；S233：继续用离子源霍尔源轰击TiN膜层表面30秒，所述轰击参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar和N2，Ar流量为10sccm、N2流量为：5sccm。
S24：在S23获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、并有离子源辅助工艺的条件下，采用高能电子束加热SiO2，以速率为将蒸发后的SiO2以纳米级分子形式沉积，获得含SiO2层的树脂镜片；离子源辅助参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar，流量为10sccm。
S25：重复S22步骤，在步骤S24获得的树脂镜片表面形成钛铌复合氧化物层；
S26：重复S21步骤，在步骤S25获得的树脂镜片表面形成硅铝复合氧化物层；
S27：重复S22步骤，在步骤S26获得的树脂镜片表面形成钛铌复合氧化物层；
S28：在S27获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、并有离子源辅助工艺的条件下，采用高能电子束加热ITO，以速率为将蒸发后的ITO以纳米级分子形式沉积，获得含ITO层的树脂镜片；
S29：在S28获得的树脂镜片表面，继续采用真空镀膜工艺，重复S21的工艺步骤，再形成一层含硅铝复合氧化物层的树脂镜片；
S3制备防水层：在S29获得的树脂镜片表面形成防水层：在S29步骤获得的镜片表面，继续采用真空镀膜工艺，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃条件下，采用高能电子束加热材料，以速率为将蒸发后的含有C12F27N的防水材料以纳米级分子形式沉积于S24获得的树脂镜片表面，即得。
实施例2
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(SK1.56-UV405)；加硬层2(VH56)/1～2.6μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/11.8nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/1.0nm，二氧化硅层3-4/35.26nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.2nm、硅铝复合氧化物层3-6/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.7nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/70.83nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)。
所述树脂镜片的制备方法所述树脂镜片的制备方法包括以下步骤：
S1：制作加硬层：将超声波清洗干净的树脂镜片基片浸入质量百分含量30％、型号为VH56的加硬液水溶液中，浸渍温度15℃，浸渍5秒后以2.0mm/s的速度提拉出溶液；80℃烘干3小时后将上述基片取出并送至烘干箱内干燥固化，固化温度120℃，固化时间150min，即得含加硬层的树脂镜片；
其余步骤同实施例1。
实施例3
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-7-UV405)；加硬层2(Z118)/1～2.6μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/14.34nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/1.0nm，二氧化硅层3-4/34.1nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/116.05nm、硅铝复合氧化物层3-6/160.78nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.34nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/70.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)。
所述树脂镜片的制备方法所述树脂镜片的制备方法包括以下步骤：
S1：制作加硬层：将超声波清洗干净的树脂镜片基片浸入质量百分含量27％、型号为Z118的加硬液水溶液中，浸渍温度15℃，浸渍5秒后以2.0mm/s的速度提拉出溶液；80℃烘干3小时后将上述基片取出并送至烘干箱内干燥固化，固化温度120℃，固化时间150min，即得含加硬层的树脂镜片；
其余步骤同实施例1。
实施例4
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/12.48nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/0.75nm，二氧化硅层3-4/34.5nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.5nm、硅铝复合氧化物层3-6/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.6nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/71.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)；
其制备方法同实施例1。
(二)对比例
对比例1
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；淡绿色防红外膜层3包括：SiO2层3-1/24.6nm、ZrO2层3-2/8.42nm、SiO2层3-3/51.42nm、ZrO2层3-4/118.72nm、SiO2层3-5/160.59nm、ZrO2层3-6/80.64nm、ITO层3-7/5nm；SiO2层3-8/66.3nm；防水层4(采用含有C12F27N的防水材料/10nm)；
其制备方法包括以下步骤：
S1：制作加硬层：将超声波清洗干净的树脂镜片基片浸入质量百分含量27％、型号为Z117的加硬液水溶液中，浸渍温度15℃，浸渍5秒后以2.0mm/s的速度提拉出溶液；80℃烘干3小时后将上述基片取出并送至烘干箱内干燥固化，固化温度120℃，固化时间150min，即得含加硬层的树脂镜片；
S2制备清底色防红外膜层：在真空镀膜机内、采用真空镀膜工艺，将固态膜层材料蒸发后经过气相传输，在S1步骤获得的树脂镜片表面沉积成薄膜，形成清底色防红外膜层，具体包括以下步骤：
S21：包括以下步骤：
S211：在S1获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内温度为60℃、无离子源辅助工艺的条件下，采用高能电子束加热SiO2，以速率为将蒸发后的SiO2以纳米级分子形式沉积，获得含第一层SiO2层的树脂镜片；
S212：在S211获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃、无离子源辅助工艺的条件下，采用高能电子束加热ZrO2，以速率为将蒸发后的ZrO2以纳米级分子形式沉积，获得含第二层ZrO2层的树脂镜片；
S213：重复S211和S212步骤，分别交替形成第三层SiO2和第四层ZrO2层以及第五层SiO2层和第六层ZrO2层，即形成包括第三层SiO2层、第四层ZrO2层、第五层SiO2层以及第六层ZrO2层的树脂镜片；
S22：在S21获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃、并有离子源辅助工艺的条件下，采用高能电子束加热ITO，以速率为将蒸发后的ITO以纳米级分子形式沉积，获得含第七层ITO层的树脂镜片；
S23：在S22获得的树脂镜片表面，继续采用真空镀膜工艺，重复S211的工艺步骤，再形成含第八层SiO2层的树脂镜片；
S3制备防水层：在S23获得的树脂镜片表面形成防水层：在S2步骤获得的镜片表面，继续采用真空镀膜工艺，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃条件下，采用高能电子束加热材料，以速率为将蒸发后的含有C12F27N的防水材料以纳米级分子形式沉积于S24获得的树脂镜片表面，即得。
对比例2
一种蓝色减反射防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；减反射层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/27.6nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/15.45nm、硅铝复合氧化物层3-3/31.42nm(材料同3-1)、钛铌复合氧化物层3-4(材料同3-2)/98.9nm、硅铝复合氧化物层3-5/171.92nm(材料同3-1)、钛铌复合氧化物层3-6(材料同3-2)/91.96nm、ITO层3-7/5nm；硅铝复合氧化物层3-8/75.8nm(材料同3-1)；防水层4(采用含有C12F27N的防水材料/10nm)；
所述树脂镜片的制备方法包括以下步骤：
S1：制作加硬层：将超声波清洗干净的树脂镜片基片浸入质量百分含量27％、型号为Z117的加硬液水溶液中，浸渍温度15℃，浸渍5秒后以2.0mm/s的速度提拉出溶液；80℃烘干3小时后将上述基片取出并送至烘干箱内干燥固化，固化温度120℃，固化时间150min，即得含加硬层的树脂镜片；
S2制备减反射防红外层：在真空镀膜机内、采用真空镀膜工艺，将固态膜层材料蒸发后经过气相传输，在S1步骤获得的树脂镜片表面沉积成薄膜，形成减反射防红外层，具体包括以下步骤：
S21：包括以下步骤：
S211：在S1获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内温度为60℃、有离子源辅助工艺的条件下，采用高能电子束加热硅铝复合氧化物，以速率为将蒸发后的硅铝复合氧化物以纳米级分子形式沉积，获得含第一层硅铝复合氧化物层的树脂镜片；
S212：在S211获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃、有离子源辅助工艺的条件下，采用高能电子束加热钛铌复合氧化物，以速率为将蒸发后的钛铌复合氧化物以纳米级分子形式沉积，获得含第二层钛铌复合氧化物层的树脂镜片；
S213：重复S211和S212步骤，分别交替形成第三层硅铝复合氧化物和第四层钛铌复合氧化物层以及第五层硅铝复合氧化物层和第六层钛铌复合氧化物层，即形成包括第三层硅铝复合氧化物层、第四层钛铌复合氧化物层、第五层硅铝复合氧化物层以及第六层钛铌复合氧化物层的树脂镜片；
S22：在S21获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃、并有离子源辅助工艺的条件下，采用高能电子束加热ITO，以速率为将蒸发后的ITO以纳米级分子形式沉积，获得含第七层ITO层的树脂镜片；
S23：在S22获得的树脂镜片表面，继续采用真空镀膜工艺，重复S211的工艺步骤，再形成含第八层硅铝复合氧化物层的树脂镜片；
S3制备防水层：在S23获得的树脂镜片表面形成防水层：在S2步骤获得的镜片表面，继续采用真空镀膜工艺，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃条件下，采用高能电子束加热材料，以速率为将蒸发后的含有C12F27N的防水材料以纳米级分子形式沉积于S24获得的树脂镜片表面，即得。
对比例3
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；减反射层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/13.48nm、硅铝复合氧化物层3-3/34.5nm(材料同3-1)、钛铌复合氧化物层3-4(材料同3-2)/114.5nm、硅铝复合氧化物层3-5/160.4nm(材料同3-1)、钛铌复合氧化物层3-6(材料同3-2)/101.62nm、ITO层3-7/5nm；硅铝复合氧化物层3-8/73nm(材料同3-1)；防水层4(采用含有C12F27N的防水材料/10nm)；
其制备工艺和方法同对比例2。
对比例4
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；减反射层3包括：SiO2层3-1/26.6nm、TiO2层3-2/13.35nm、SiO2层3-3/34.8nm、TiO2层3-4/113.81nm、SiO2层3-5/161.65nm、TiO2层3-6/101.11nm、ITO层3-7/5nm；SiO2层3-8/73.6nm；防水层4(采用含C12F27N的防水材料/10nm)；其制备方法包括以下步骤：
S1：制作加硬层：将超声波清洗干净的树脂镜片基片浸入质量百分含量27％、型号为Z117的加硬液水溶液中，浸渍温度15℃，浸渍5秒后以2.0mm/s的速度提拉出溶液；80℃烘干3小时后将上述基片取出并送至烘干箱内干燥固化，固化温度120℃，固化时间150min，即得含加硬层的树脂镜片；
S2制备清底色防红外膜层：在真空镀膜机内、采用真空镀膜工艺，将固态膜层材料蒸发后经过气相传输，在S1步骤获得的树脂镜片表面沉积成薄膜，形成清底色防红外膜层，具体包括以下步骤：
S21：包括以下步骤：
S211：在S1获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内温度为60℃、有离子源辅助工艺的条件下，采用高能电子束加热SiO2，以速率为将蒸发后的SiO2以纳米级分子形式沉积，获得含第一层SiO2层的树脂镜片；
S212：在S211获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃、有离子源辅助工艺的条件下，采用高能电子束加热TiO2，以速率为将蒸发后的TiO2以纳米级分子形式沉积，获得含第二层TiO2层的树脂镜片；
S213：重复S211和S212步骤，分别交替形成第三层SiO2层和第四层TiO2层以及第五层SiO2层和第六层TiO2层，即形成包括第三层SiO2层、第四层TiO2层、第五层SiO2层以及第六层TiO2层的树脂镜片；
S22：在S21获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃、并有离子源辅助工艺的条件下，采用高能电子束加热ITO，以速率为将蒸发后的ITO以纳米级分子形式沉积，获得含第七层ITO层的树脂镜片；
S23：在S22获得的树脂镜片表面，继续采用真空镀膜工艺，重复S211的工艺步骤，再形成含第八层SiO2层的树脂镜片；
S3制备防水层：在S23获得的树脂镜片表面形成防水层：在S2步骤获得的镜片表面，继续采用真空镀膜工艺，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为60℃条件下，采用高能电子束加热材料，以速率为将蒸发后的含有C12F27N的防水材料以纳米级分子形式沉积于S24获得的树脂镜片表面，即得。
对比例5
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/12.48nm、SiO-Cr吸收层3-3(SiO:Cr摩尔比为1:1，由丹阳市科达镀膜材料有限公司烧结)/1.2nm，二氧化硅层3-4/34.5nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.5nm、硅铝复合氧化物层3-6/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.6nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/71.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)；
其制备方法除了3-3层SiO-Cr吸收层以外，其他工艺与实施例1相同。
SiO-Cr吸收层的制备工艺为：在步骤S22获得的树脂镜片表面形成SiO-Cr层。先抽真空至本底真空度≤1.2×10-4Pa。然后在离子源霍尔源辅助工艺下沉积，采用高能电子束加热SiO-Cr，以速率将蒸发的SiO-Cr以纳米级分子形式沉积，获得含SiO-Cr层的树脂镜片。这里离子源辅助参数为：阳极电压：110V，阳极电流：3A，Ar流量为12sccm。
对比例6
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/12.48nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/1.0nm，二氧化硅层3-4/34.5nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.5nm、硅铝复合氧化物层3-6/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.6nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/71.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)；
其制备方法除了3-3层氮化钛以外，其他工艺与实施例1相同。
氮化钛的制备工艺为：在步骤S22获得的树脂镜片表面形成氮化钛层。先抽真空至本底真空度≤8×10-4Pa。再用离子源霍尔源轰击60秒，离子源轰击参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar，流量为10sccm。然后在离子源霍尔源辅助工艺下沉积，采用高能电子束加热TiN，以速率将蒸发的TiN以纳米级分子形式沉积，获得含TiN层的树脂镜片。这里离子源辅助参数为：阳极电压：110V，阳极电流：3A，Ar流量为12sccm,无氮气流量。得到含TiN层的树脂镜片，继续用离子源轰击TiN表面30秒，其离子源参数与本层离子源辅助参数相同。
对比例7
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/12.48nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/1.0nm，二氧化硅层3-4/34.5nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.5nm、硅铝复合氧化物层3-6/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.6nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/71.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)；
其制备方法除了3-3层氮化钛以外，其他工艺与实施例1相同。氮化钛的制备工艺为：S23：在步骤S22获得的树脂镜片表面形成氮化钛层。先抽真空至本底真空度≤8×10-4Pa。无离子源霍尔源预轰击。直接在离子源霍尔源辅助工艺下沉积，采用高能电子束加热TiN，以速率将蒸发的TiN以纳米级分子形式沉积，获得含TiN层的树脂镜片。这里离子源辅助参数为：阳极电压：110V，阳极电流：3A，Ar流量为10sccm,氮气流量为：5sccm。得到含TiN层的树脂镜片，继续用离子源轰击TiN表面30秒，其离子源参数与本层离子源辅助参数相同
对比例8
一种清底色防红外树脂镜片，依次排列包括：树脂镜片基片1(MR-8-UV405)；加硬层2(Z117)/2.6～3μm；清底色防红外膜层3包括：硅铝复合氧化物层3-1(其中SiO2和Al2O3摩尔量百分比：92％SiO2：8％Al2O3；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为SA56)/26nm、钛铌复合氧化物层3-2(其中TiO2和Nb2O5摩尔量百分比为：80％TiO2：20％Nb2O5；委托常州市瞻驰光电科技股份有限公司开发并生产，材料型号为PTN28)/12.48nm、氮化钛层3-3(分子式TiN，纯度99.9％以上，由常州瞻驰光电科技股份有限公司烧结)/1.0nm，二氧化硅层3-4/34.5nm(分子式SiO2,纯度99.99％，由丹阳市科达镀膜材料有限公司烧结)、钛铌复合氧化物层3-5(材料同3-2)/114.5nm、硅铝复合氧化物层3-6/160.4nm(材料同3-1)；钛铌复合氧化物层3-7(材料同3-2)/101.6nm；ITO层3-8/5nm；硅铝复合氧化物层3-9/71.0nm(材料同3-1)；防水层4(采用含C12F27N的防水材料/10nm)；
其制备方法除了3-3层氮化钛以外，其他工艺与实施例1相同。
氮化钛的制备工艺为S23：在步骤S22获得的树脂镜片表面形成氮化钛层。先抽真空至本底真空度≤3×10-3Pa(并不专门控制真空)。再用离子源霍尔源轰击60秒，离子源轰击参数为：阳极电压：110V，阳极电流：3A，辅助气为Ar，流量为10sccm。然后在离子源霍尔源辅助工艺下沉积，采用高能电子束加热TiN，以速率将蒸发的TiN以纳米级分子形式沉积，获得含TiN层的树脂镜片。这里离子源辅助参数为：阳极电压：110V，阳极电流：3A，Ar流量为10sccm,氮气流量为：5sccm。得到含TiN层的树脂镜片，继续用离子源轰击TiN表面30秒，其离子源参数与本层离子源辅助参数相同。
二、实验例
主要实施例和对比例材料清单如下，含TiN或SiO-Cr的为9层的防红外膜层结构，不含的为8层防红外膜系。
表1.实施例和对比例材料比较
1.测定镜片的平均反射率、透射率、黄色指数和防红外效果
1.1测定实施例1～4和对比例1～8平均反射率、透过率和防红外效果
对实施例1～4以及对比例1～8制备获得的镜片，测定其平均反射率(平均反射率：是指在C光(CIE中定义的色温6774K的光源)照明下的视觉平均反射率，在这里指单面的反射率)，平均透过率(平均透过率：是指在C光(CIE中定义的色温6774K的光源)照明下的视觉平均透过率，在这里指双面镀制同样膜系的透过率)，黄色指数(指双面镀好后，参照QB-T-2506-2001计算的镜片黄色指数)及近红外的透过率(近红外平均透过率：这里指双面镀好后，参照QB-T-2506-2017计算的镜片近红外截止率)，测量结果记录在如下表2中：
表2.反射率、红外阻隔率和黄色指数对比
从对比例2和对比例3可见，绿膜的防红外工艺红外阻隔率更高，黄色指数更低。采用了专门工艺的TiN层，红外阻隔率进一步提升，黄色指数进一步下降。镜片目视效果更为清透。
1.2测定镜片的防蓝光效果
参照国标GB/T38120—2019，检查镜片是否符合标准。
表3.防蓝光指标和黄色指数对比
1.3对比TiN工艺对防蓝光标准和黄色指数的影响
测试单面的透射反射，折算出吸收的结果如下：
表4.TiN工艺对防蓝光指标和黄色指数的影响
一般工艺采用SiO-Cr作为吸收层，能够有效满足防蓝光的需求。但是其黄绿光吸收较低，会导致黄色指数增高。大部分弱吸收材料都是这个特性。
严格控制TiN膜层的制备工艺，有助于制备膜层达到预期技术效果。(1)当TiN在真空控制不严时，会有氧化的趋势，从而降低膜层吸收，并对黄绿光和红外光吸收下降的更快，从而导致黄色指数上升，镜片目视发黄不清透；(2)当TiN不用离子源辅助时，膜层疏松，并会在蒸发过程中降低氮含量，在镀其他层时会补充氧化。从而出现氧化的趋势，从而降低膜层吸收，并对黄绿光和红外光吸收下降的更快，从而导致黄色指数上升，镜片目视发黄不清透；(3)当TiN离子源辅助时不用氮气辅助，会导致膜层的金属化(氮化不足)，吸收急剧增加。蓝光的吸收增加的比黄绿光和红外快的多，从而导致黄色指数上升，镜片目视发黄发灰不清透。采用本发明特定工艺制备TiN层，能够有效增加近红外的阻隔吸收，控制蓝光吸收，并增加黄光吸收，从而降低黄色指数，使镜片更为清透美观。
2.耐高温、耐久性和高温附着力测试
2.1耐温实验：
完成样品(实施例1～4以及对比例1～8)后，存放一周后测试了样品的耐温性能。耐温性能的测试方法是参照国家树脂镜片耐温标准(GB10810.4-2012)中的第5.8条款：通过55℃30分钟的烘烤测试。通过后同样的方法每次增加5℃烘烤30分钟测试，直到镜片出现膜裂或橘皮等失效现象，并记录合格的最高温度。结果记录在如下表5中。
2.2高温附着力实验：
附着力测试指参照国标GB10810.4～2012中第5.9条的膜层附着力测试。高温膜层附着力测试是指万新公司参照国标GB10810.4～2012中第5.9条，将水煮条件改成90±2℃60分钟，其他测试方法都一样。附着力和高温附着力测试结果：等级A指的是不脱膜或脱膜面积小于5％，等级B指脱膜面积在5％～15％之间，等级C(不合格)指脱膜面积明显大于15％。为验证产品附着力分布，从镀膜室中5个不同位置做了高温附着力测试。实施例1～4以及对比例1～8的测试结果记录在如下表5中。
2.3高温高湿测试
光伏行业和光通讯行业用高温高湿来评估产品的耐久性。参照光伏行业测试标准(GB/T 18911-2002,IEC61646:1996的第10.13条)和光通讯行业(Ballcore Test,GR-1221-Core第6.2.5条)的测试方法，定义树脂镜片耐高温高湿测试调试为：85℃、85％湿度下的存储12小时，查看制备镜片是否存在膜裂或橘皮等明显失效现象；每次高温高湿测试放入不同位置的3片树脂镜片。实施例1～4以及对比例1～8的测试结果记录在如下表5中。
表5耐高温、耐久性和高温附着力测试结果
由此可见，在其他条件不变的情况下，镜片高折射率材料采用钛铌复合氧化物的耐高温性能、高温附着力、耐久性比其他常规材料更好；低折射率材料采用硅铝复合氧化物的耐高温性能、高温附着力、耐久性比其他常规材料更好；我们采用这两种特定配比材料制备膜系及其恰当的工艺以保证清底色防红外产品的耐高温性和耐久性。

Claims (17)

  1. 一种清底色防蓝光防红外耐高温的树脂镜片，其特征在于，包括：树脂镜片基片、加硬层以及清底色防红外层；其中，所述树脂镜片基片、加硬层以及清底色防红外膜层依次排列，所述加硬层位于所述树脂镜片基片表面，所述清底色防红外膜层位于所述加硬层表面。
  2. 根据权利要求1所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述清底色防红外耐高温的树脂镜片还包括防水层，所述防水层位于所述清底色防红外膜层表面。
  3. 根据权利要求1所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述加硬层的材料为有机硅；进一步优选的，所述有机硅中至少含有Ti元素。
  4. 根据权利要求1所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述清底色防红外膜层包括硅铝复合氧化物层、钛铌复合氧化物层、掺锡氧化铟(即ITO)层以及氮化钛(TiN)层；更进一步的，所述清底色防红外膜层包括三层硅铝复合氧化物层、三层钛铌复合氧化物层、一层掺锡氧化铟(即ITO)层、一层二氧化硅层以及一层氮化钛(TiN)。
  5. 根据权利要求4所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述硅铝复合氧化物层由SiO2和Al2O3复合材料组成，且其中SiO2占所述复合材料的摩尔分数为70％～95％；进一步优选的，其中SiO2占所述复合材料摩尔分数的92％。
  6. 根据权利要求4所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述钛铌复合氧化物层由TiO2和Nb2O5复合材料组成，其中TiO2占所述复合材料摩尔分数的10％～90％；优选的，其中TiO2占所述复合材料摩尔分数的80％。
  7. 根据权利要求4所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述氮化钛层中TiN纯度大于99.9wt％。
  8. 根据权利要求1所述的清底色防蓝光防红外耐高温的树脂镜片， 其特征在于，所述加硬层的厚度为1～5μm。
  9. 根据权利要求1所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述清底色防红外膜层的厚度为290～950nm。
  10. 根据权利要求2所述的清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述防水层的厚度为4～20nm。
  11. 根据权利要求1～10任一项所述清底色防蓝光防红外耐高温的树脂镜片，其特征在于，所述清底色防蓝光防红外树脂耐高温镜片的平均反射率≤1.5％。
  12. 根据权利要求1～10任一项所述清底色防蓝光防红外耐高温的树脂镜片，所述清底色防蓝光防红外树脂耐高温镜片的近红外阻隔率＞55％。
  13. 根据权利要求1～10任一项所述清底色防蓝光防红外耐高温的树脂镜片，所述清底色防蓝光防红外树脂耐高温镜片的黄色指数≤4.5％。
  14. 一种权利要求1～10任一项所述清底色防蓝光防红外树脂耐高温镜片的制备方法，其特征在于，包括以下步骤：
    S1制备加硬层：在树脂镜片基片表面形成加硬层，即获得含加硬层的树脂镜片；
    S2制备清底色防红外膜层：在S1获得的树脂镜片表面形成所述清底色防红外膜层，即获得含清底色防红外膜层的树脂镜片，具体包括：
    S21：在步骤S1获得的树脂镜片表面分别形成含第一层硅铝复合氧化物层、第二层钛铌复合氧化物层的树脂镜片；
    S22：在步骤S21获得的树脂镜片表面形成第三层含氮化钛层的树脂镜片；
    S23：在步骤S22获得的树脂镜片表面形成第四层含SiO2层的树脂镜片；
    S24：在步骤S23获得的树脂镜片表面形成分别形成第五层钛铌复合氧化物层、第六层硅铝复合氧化物层以及第七层钛铌复合氧化物层的树脂镜片。
    S25：在步骤S24获得的树脂镜片表面形成含形成第八层含ITO层的树脂镜片；
    S26：在步骤S25获得的树脂镜片表面再形成第九层含硅铝复合氧化物层的树脂镜片；
    S3制备防水层：在步骤S2获得的树脂镜片表面形成防水层。
  15. 根据权利要求14所述清底色防蓝光防红外树脂耐高温镜片的制备方法，其特征在于，所述S1制备加硬层的步骤包括：将超声波清洗干净的树脂镜片基片浸入质量百分含量25～30％的加硬液水溶液中，浸渍温度10～20℃，浸渍4～8秒后以1.0～3.0mm/s的速度提拉出溶液，再将其于70～90℃烘干2～5小时后将上述基片取出并送至烘干箱内干燥固化，固化温度100～150℃，固化时间120～180min，即得含加硬层的树脂镜片。
  16. 根据权利要求14所述清底色防蓝光防红外树脂耐高温镜片的制备方法，其特征在于，所述步骤S2制备清底色防红外膜层的工艺包括：在真空镀膜机内、采用真空镀膜工艺，将硅铝复合氧化物层、钛铌复合氧化物、氮化钛、二氧化硅以及ITO固态膜层材料蒸发后经过气相传输，在S1步骤获得的树脂镜片表面沉积成薄膜，形成清底色防红外膜层，具体包括以下步骤：
    S21：在步骤S1获得的树脂镜片表面形成第一层硅铝复合氧化物层，在本底真空度≤3×10-3Pa、且镀膜舱内温度为50～70℃、有离子源辅助工艺的条件下，采用高能电子束加热所述硅铝复合氧化物，以速率为将蒸发后的硅铝复合氧化物以纳米级分子形式沉积，获得含第一层硅铝复合氧化物层的树脂镜片；
    S22：在步骤S21获得的树脂镜片表面形成钛铌复合氧化物层，在S21获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、有离子源辅助工艺的条件下，采用高能电子束加热所述钛铌复合氧化物，以速率为将蒸发后的钛铌复合氧化物以纳米级分子形式沉积，获得含第二层钛铌复合氧化物层的树脂镜片；
    S23：在步骤S22获得的树脂镜片表面形成氮化钛层，具体包括：
    S231：先抽真空至本底真空度≤8×10-4Pa，再用离子源霍尔源轰击50～80秒，离子源轰击参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar，流量为5～20sccm；
    S232：在离子源辅助工艺下沉积，采用高能电子束加热TiN，以速率将蒸发的TiN以纳米级分子形式沉积，所述离子源辅助参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar和N2，Ar流量为5～15sccm、N2流量为：3～15sccm；
    S233：继续用离子源霍尔源轰击TiN膜层表面20～40秒，所述轰击参数为：阳极电压：90～140V，阳极电流：2.5～5A，辅助气为Ar和N2，Ar流量为5～15sccm、N2流量为：3～15sccm；
    S24：在S23获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、并有离子源辅助工艺的条件下，采用高能电子束加热SiO2，以速率为将蒸发后的SiO2以纳米级分子形式沉积，获得含SiO2层的树脂镜片；
    S25：重复S22步骤，在步骤S24获得的树脂镜片表面形成钛铌复合氧化物层；
    S26：重复S21步骤，在步骤S25获得的树脂镜片表面形成硅铝复合氧化物层；
    S27：重复S22步骤，在步骤S26获得的树脂镜片表面形成钛铌复合氧化物层；
    S28：在S27获得的树脂镜片表面，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃、并有离子源辅助工艺的条件下，采用高能电子束加热ITO，以速率为将蒸发后的ITO以纳米级分子形式沉积，获得含ITO层的树脂镜片；
    S29：在S28获得的树脂镜片表面，继续采用真空镀膜工艺，重复S21的工艺步骤，再形成一层含硅铝复合氧化物层的树脂镜片。
  17. 根据权利要求14所述清底色防蓝光防红外树脂耐高温镜片的制备方法，其特征在于，所述步骤S3中，在S2获得的树脂镜片表面形成防水层包括以下步骤：在S29步骤获得的镜片表面，继续采用真空镀膜工艺，在本底真空度≤3×10-3Pa、且镀膜舱内的温度为50～70℃条件下,采用高能电子束加热材料，以速率为将蒸发后的含氟防水材料以纳米级分子形式进行沉积，获得含防水层的树脂镜片。
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