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WO2020042207A1 - Ultraviolet light prevention night vision compatible thin film material and preparation method therefor - Google Patents

Ultraviolet light prevention night vision compatible thin film material and preparation method therefor Download PDF

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Publication number
WO2020042207A1
WO2020042207A1 PCT/CN2018/104309 CN2018104309W WO2020042207A1 WO 2020042207 A1 WO2020042207 A1 WO 2020042207A1 CN 2018104309 W CN2018104309 W CN 2018104309W WO 2020042207 A1 WO2020042207 A1 WO 2020042207A1
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night vision
film material
film
compatible
mass
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Chinese (zh)
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王丽熙
张其土
管永康
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Suzhou Xunneng Optoelectronic Technology Co Ltd
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Suzhou Xunneng Optoelectronic Technology Co Ltd
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    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/20Filters
    • G02B5/208Filters for use with infrared or ultraviolet radiation, e.g. for separating visible light from infrared and/or ultraviolet radiation
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00Optical elements other than lenses
    • G02B5/20Filters
    • G02B5/22Absorbing filters
    • G02B5/223Absorbing filters containing organic substances, e.g. dyes, inks or pigments

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  • the invention belongs to the field of thin film materials, and relates to an anti-ultraviolet night vision compatible thin film material and a preparation method thereof.
  • Night vision compatible technology refers to the elimination of light and radiation from the cockpit lighting system that interfere with the night vision device's work through certain technical means, thereby ensuring the normal operation of the night vision device.
  • the use of near-infrared absorbing materials to absorb disturbing light is an important means to achieve night vision compatible technology.
  • the aircraft cockpit lighting system has undergone continuous changes in the red, blue and white, and white lighting systems.
  • these lighting systems use visually visible light such as incandescent lamps or ordinary light emitting diodes as light sources, and they have high spectral energy radiation in the near infrared region. This area is the spectral response area of night vision products such as night vision goggles.
  • the current lighting system must be improved to suit the NVIS environment, that is, night vision compatible technology.
  • the film material with night vision compatibility has very wide application prospects.
  • the properties of different thin film materials also have large differences, so how to prepare thin film materials with good UV protection and high transmittance has become a research problem.
  • the conventional anti-ultraviolet light is also compatible with thin film materials. Its anti-ultraviolet performance is poor, and its transmittance in the visible light region is low, which cannot meet the needs of practical use.
  • the present invention discloses an anti-ultraviolet night vision compatible thin film material.
  • the thin film material includes a layer of 25nm to 200nm transparent substrate and 5nm to 20nm coated on the transparent substrate. UV-resistant night vision compatible coating;
  • the transparent substrate is a polyethylene terephthalate film, a polybutylene terephthalate film, a polyethylene naphthalate film, a polycarbonate film, a polypropylene film, a polyimide film, or Polyamide film.
  • the raw materials and components of the anti-ultraviolet night vision compatible coating layer are as follows: 0.3-0.8 parts by mass of an ultraviolet absorber, 0.1-0.5 parts by mass of a near-infrared absorber, and 100 parts by mass of a matrix resin.
  • the resin curing agent is 10 to 25 parts by mass, and the organic solvent is 30 to 50 parts by mass.
  • the ultraviolet absorber is benzotriazole UV-360, benzotriazole UV-326 or benzophenone UV-531.
  • the near-infrared absorbing agent is one or more of a thiodiene-type nickel dye, a methylcyanine dye, and a phthalocyanine dye.
  • the matrix resin is polymethyl methacrylate or polycarbonate.
  • the resin curing agent is an aliphatic polyisocyanate or an alicyclic polyisocyanate
  • the organic solvent is chloroform, dichloromethane, or acetone.
  • a method for preparing a UV-resistant night vision compatible film material the specific steps are as follows:
  • step (3) The film obtained in step (2) is dried for 4 to 6 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for curing for 5 to 8 hours.
  • the obtained thin film material After the anti-ultraviolet night vision compatible coating prepared by the present invention is prepared through a special process and a specific blending range, the obtained thin film material has a good transmittance in the visible light region, and its anti-ultraviolet performance is also very good. Well, it has a very broad application prospect.
  • FIG. 1 is a transmission spectrum of a thin film material prepared according to the present invention.
  • step (3) The film obtained in step (2) is dried for 4 hours. After the solvent is volatilized, it is transferred to an oven at 80 ° C. for curing for 7 hours.
  • step (3) The film obtained in step (2) is dried for 6 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for 6 hours to be cured.
  • step (3) The film obtained in step (2) is dried for 6 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for 7 hours for curing.
  • step (3) The film obtained in step (2) is dried for 4 hours. After the solvent is evaporated, it is transferred to an 80 ° C oven for 5 hours to be cured.
  • step (3) The film obtained in step (2) is dried for 5 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for 8 hours.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
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Abstract

An ultraviolet light prevention night vision compatible thin film material and a preparation method therefor. The thin film material is divided into two layers, wherein one layer is a transparent substrate, and the other layer is a near-infrared absorbing film layer having ultraviolet light prevention ability. The film material has strong absorption characteristics in the wavelength ranges of 320 nm-400 nm and 650 nm-930 nm, and has a high transmittance in the visible light range of 440 nm-625 nm. The present invention has a broad application prospect.

Description

一种防紫外光夜视兼容薄膜材料及其制备方法Anti-ultraviolet night vision compatible film material and preparation method thereof 技术领域Technical field

本发明属于薄膜材料领域,本发明涉及一种防紫外光夜视兼容薄膜材料及其制备方法。The invention belongs to the field of thin film materials, and relates to an anti-ultraviolet night vision compatible thin film material and a preparation method thereof.

背景技术Background technique

夜视兼容技术是指通过一定技术手段消除座舱内照明系统发出的干扰夜视仪工作的光和辐射,从而确保夜视仪的正常工作。采用近红外吸收材料吸收干扰光是实现夜视兼容技术的重要手段。目前,飞机座舱照明系统经历了红光、兰白光、白光照明体制的不断变革。但是这些照明体制均采用白炽灯或普通发光二极管等目视可见光作为光源,他们在近红外区有较高的光谱能量辐射。而这个区域正是夜视镜等夜视产品光谱响应区域,在夜视模式下,势必对夜视成像系统(NVIS)造成干扰,严重影响成像效果,甚至无法辨认图像。因此必须对现行的照明体制进行改进,以适应NVIS使用环境,也就是夜视兼容技术。而具有夜视兼容功能的薄膜材料就具有非常广泛的应用前景。不同薄膜材料的性能也有较大的差异,因此如何制备具有良好防紫外功能、还能具有较高的透过率的薄膜材料成为研究的难题。Night vision compatible technology refers to the elimination of light and radiation from the cockpit lighting system that interfere with the night vision device's work through certain technical means, thereby ensuring the normal operation of the night vision device. The use of near-infrared absorbing materials to absorb disturbing light is an important means to achieve night vision compatible technology. At present, the aircraft cockpit lighting system has undergone continuous changes in the red, blue and white, and white lighting systems. However, these lighting systems use visually visible light such as incandescent lamps or ordinary light emitting diodes as light sources, and they have high spectral energy radiation in the near infrared region. This area is the spectral response area of night vision products such as night vision goggles. Under night vision mode, it will inevitably cause interference to the night vision imaging system (NVIS), seriously affect the imaging effect, and even fail to recognize the image. Therefore, the current lighting system must be improved to suit the NVIS environment, that is, night vision compatible technology. The film material with night vision compatibility has very wide application prospects. The properties of different thin film materials also have large differences, so how to prepare thin film materials with good UV protection and high transmittance has become a research problem.

发明内容Summary of the Invention

要解决的技术问题:常规的防紫外光也是兼容薄膜材料其防紫外光的性能较差,并且其在可见光区域透过率较低,其并不能满足实际使用的需要。Technical problem to be solved: The conventional anti-ultraviolet light is also compatible with thin film materials. Its anti-ultraviolet performance is poor, and its transmittance in the visible light region is low, which cannot meet the needs of practical use.

技术方案:为了解决上述问题,本发明公开了一种防紫外光夜视兼容薄膜材料,所述的薄膜材料包括一层25nm~200nm的透明基材以及涂覆在透明基材上的5nm~20nm的防紫外光夜视兼容涂层;Technical solution: In order to solve the above problems, the present invention discloses an anti-ultraviolet night vision compatible thin film material. The thin film material includes a layer of 25nm to 200nm transparent substrate and 5nm to 20nm coated on the transparent substrate. UV-resistant night vision compatible coating;

所述透明基材为聚对苯二甲酸乙二酯薄膜、聚对苯二甲酸丁二酯薄膜、聚萘二甲酸亚乙酯薄膜、聚碳酸酯薄膜、聚丙烯薄膜、聚酰亚胺薄膜或聚酰胺薄膜。The transparent substrate is a polyethylene terephthalate film, a polybutylene terephthalate film, a polyethylene naphthalate film, a polycarbonate film, a polypropylene film, a polyimide film, or Polyamide film.

优选的,所述防紫外光夜视兼容涂层涂层其原料及各组分质量份如下:紫外吸收剂0.3-0.8质量份,近红外吸收剂0.1~0.5质量份,基体树脂100质量份,树脂固化剂10~25质量份,有机溶剂30~50质量份。Preferably, the raw materials and components of the anti-ultraviolet night vision compatible coating layer are as follows: 0.3-0.8 parts by mass of an ultraviolet absorber, 0.1-0.5 parts by mass of a near-infrared absorber, and 100 parts by mass of a matrix resin. The resin curing agent is 10 to 25 parts by mass, and the organic solvent is 30 to 50 parts by mass.

优选的,所述紫外吸收剂为苯并三唑UV-360、苯并三唑UV-326或二苯甲酮UV-531。Preferably, the ultraviolet absorber is benzotriazole UV-360, benzotriazole UV-326 or benzophenone UV-531.

优选的,所述近红外吸收剂为硫代双烯型镍染料、甲基菁类染料和酞菁类染料中的一种或多种。Preferably, the near-infrared absorbing agent is one or more of a thiodiene-type nickel dye, a methylcyanine dye, and a phthalocyanine dye.

优选的,所述基体树脂为聚甲基丙烯酸甲酯或聚碳酸酯。Preferably, the matrix resin is polymethyl methacrylate or polycarbonate.

优选的,所述树脂固化剂为脂肪类聚异氰酸酯或脂环类聚异氰酸酯,所述有机溶剂为氯仿、二氯甲烷或丙酮。Preferably, the resin curing agent is an aliphatic polyisocyanate or an alicyclic polyisocyanate, and the organic solvent is chloroform, dichloromethane, or acetone.

一种防紫外光夜视兼容薄膜材料的制备方法,其具体步骤如下:A method for preparing a UV-resistant night vision compatible film material, the specific steps are as follows:

(1)将透明基材表面清洗干净;(1) Clean the surface of the transparent substrate;

(2)按比例称取防紫外光夜视兼容涂层的各原料,溶于有机溶剂中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤(1)所得透明基材表面;(2) Weigh each raw material of the UV-resistant night vision-compatible coating in proportion and dissolve it in an organic solvent to prepare a UV-resistant night-vision compatible coating, and apply the coating on the surface of the transparent substrate obtained in step (1). ;

(3)将步骤(2)中所得薄膜干燥4~6小时,待溶剂挥发后后转移至80℃烘箱固化5~8小时。(3) The film obtained in step (2) is dried for 4 to 6 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for curing for 5 to 8 hours.

有益效果:本发明制备的防紫外光夜视兼容涂层通过特殊的工艺及特定的配比范围制备后,得到的薄膜材料在可见光区域有较好的透过率,并且其防紫外性能也非常好,具有非常广的应用前景。Beneficial effect: After the anti-ultraviolet night vision compatible coating prepared by the present invention is prepared through a special process and a specific blending range, the obtained thin film material has a good transmittance in the visible light region, and its anti-ultraviolet performance is also very good. Well, it has a very broad application prospect.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1是为本发明制备的薄膜材料的透射光谱。FIG. 1 is a transmission spectrum of a thin film material prepared according to the present invention.

具体实施方式detailed description

实施例1Example 1

(1)将透明基材聚对苯二甲酸乙二酯薄膜表面清洗干净;(1) Clean the surface of the transparent substrate polyethylene terephthalate film;

(2)取紫外吸收剂苯并三唑UV-360为0.3质量份,近红外吸收剂硫代双烯型镍染料0.5质量份,基体树脂聚甲基丙烯酸甲酯100质量份,树脂固化剂脂肪类聚异氰酸酯10质量份,溶于30重量份有机溶剂氯仿中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤(1)所得透明基材表面;(2) 0.3 parts by mass of benzotriazole UV-360, 0.5 parts by mass of thiodiene type nickel dye of near-infrared absorber, 100 parts by mass of polymethyl methacrylate as matrix resin, and fat of resin curing agent 10 parts by mass of a polyisocyanate-like compound, dissolved in 30 parts by weight of an organic solvent, chloroform, to obtain an anti-ultraviolet night vision compatible coating, and coating the coating on the surface of the transparent substrate obtained in step (1);

(3)将步骤(2)中所得薄膜干燥4小时,待溶剂挥发后后转移至80℃烘箱固化7小时。(3) The film obtained in step (2) is dried for 4 hours. After the solvent is volatilized, it is transferred to an oven at 80 ° C. for curing for 7 hours.

实施例2Example 2

(1)将透明基材聚对苯二甲酸丁二酯薄膜表面清洗干净;(1) Clean the surface of the transparent substrate polybutylene terephthalate film;

(2)取紫外吸收剂苯并三唑UV-326为0.8质量份,近红外吸收剂甲基菁类染料0.1质量份,基体树脂聚甲基丙烯酸甲酯100质量份,树脂固化剂脂肪类聚异氰酸酯25质量份,溶于50重量份有机溶剂二氯甲烷中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤(1)所得透明基材表面;(2) Take 0.8 mass parts of benzotriazole UV-326 as ultraviolet absorber, 0.1 mass parts of methyl cyanine dye as near-infrared absorber, 100 mass parts of polymethyl methacrylate as matrix resin, and fatty polymer as resin curing agent. 25 parts by mass of isocyanate was dissolved in 50 parts by weight of organic solvent dichloromethane to prepare an ultraviolet night vision-resistant coating, and the coating was applied on the surface of the transparent substrate obtained in step (1);

(3)将步骤(2)中所得薄膜干燥6小时,待溶剂挥发后后转移至80℃烘箱固化6小时。(3) The film obtained in step (2) is dried for 6 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for 6 hours to be cured.

实施例3Example 3

(1)将透明基材聚萘二甲酸亚乙酯薄膜表面清洗干净;(1) Clean the surface of the transparent substrate polyethylene naphthalate film;

(2)取紫外吸收剂二苯甲酮UV-531为0.2质量份,近红外吸收剂酞 菁类染料0.3质量份,基体树脂聚甲基丙烯酸甲酯100质量份,树脂固化剂脂肪类聚异氰酸酯15质量份,溶于30重量份有机溶剂氯仿中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤(1)所得透明基材表面;(2) 0.2 parts by mass of benzophenone UV-531 as an ultraviolet absorber, 0.3 parts by mass of a near-infrared absorber phthalocyanine dye, 100 parts by mass of a base resin polymethyl methacrylate, and a resin curing agent fatty polyisocyanate 15 parts by mass, dissolved in 30 parts by weight of an organic solvent, chloroform, to obtain an anti-ultraviolet night vision compatible coating, and coating the coating on the surface of the transparent substrate obtained in step (1);

(3)将步骤(2)中所得薄膜干燥6小时,待溶剂挥发后后转移至80℃烘箱固化7小时。(3) The film obtained in step (2) is dried for 6 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for 7 hours for curing.

实施例4Example 4

(1)将透明基材聚碳酸酯薄膜表面清洗干净;(1) Clean the surface of the polycarbonate film on the transparent substrate;

(2)取紫外吸收剂苯并三唑UV-360为0.6质量份,近红外吸收剂酞菁类染料0.2质量份,基体树脂聚甲基丙烯酸甲酯100质量份,树脂固化剂脂肪类聚异氰酸酯20质量份,溶于50重量份有机溶剂二氯甲烷中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤(1)所得透明基材表面;(2) Take 0.6 mass parts of benzotriazole UV-360 as ultraviolet absorber, 0.2 mass parts of phthalocyanine dye as near-infrared absorber, 100 mass parts of polymethyl methacrylate as matrix resin, and fatty polyisocyanate as resin curing agent. 20 parts by mass, dissolved in 50 parts by weight of an organic solvent, methylene chloride, to obtain an ultraviolet night vision-resistant coating, and coating the coating on the surface of the transparent substrate obtained in step (1);

(3)将步骤(2)中所得薄膜干燥4小时,待溶剂挥发后后转移至80℃烘箱固化5小时。(3) The film obtained in step (2) is dried for 4 hours. After the solvent is evaporated, it is transferred to an 80 ° C oven for 5 hours to be cured.

实施例5Example 5

(1)将透明基材聚丙烯薄膜表面清洗干净;(1) Clean the surface of the transparent substrate polypropylene film;

(2)取紫外吸收剂苯并三唑UV-326为0.5质量份,近红外吸收剂硫代双烯型镍染料0.4质量份,基体树脂聚甲基丙烯酸甲酯100质量份,树脂固化剂脂肪类聚异氰酸酯25质量份,溶于40重量份有机溶剂丙酮中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤(1)所得透明基材表面;(2) Take 0.5 mass parts of benzotriazole UV-326 as ultraviolet absorber, 0.4 mass parts of thiodiene type nickel dye as near-infrared absorber, 100 mass parts of polymethyl methacrylate as matrix resin, and resin curing agent as fat 25 parts by mass of a polyisocyanate-like compound, dissolved in 40 parts by weight of an organic solvent, acetone, to obtain an anti-ultraviolet night vision compatible coating, and coating the coating on the surface of the transparent substrate obtained in step (1);

(3)将步骤(2)中所得薄膜干燥5小时,待溶剂挥发后后转移至80℃烘箱固化8小时。(3) The film obtained in step (2) is dried for 5 hours. After the solvent is volatilized, it is transferred to an 80 ° C oven for 8 hours.

Claims (7)

一种防紫外光夜视兼容薄膜材料,其特征在于:所述的薄膜材料包括一层25nm~200nm的透明基材以及涂覆在透明基材上的5nm~20nm的防紫外光夜视兼容涂层;A UV-resistant night vision-compatible film material, characterized in that the film material includes a layer of 25nm to 200nm transparent substrate and a 5nm to 20nm UV-proof night vision compatible coating coated on the transparent substrate. Floor; 所述透明基材为聚对苯二甲酸乙二酯薄膜、聚对苯二甲酸丁二酯薄膜、聚萘二甲酸亚乙酯薄膜、聚碳酸酯薄膜、聚丙烯薄膜、聚酰亚胺薄膜或聚酰胺薄膜。The transparent substrate is a polyethylene terephthalate film, a polybutylene terephthalate film, a polyethylene naphthalate film, a polycarbonate film, a polypropylene film, a polyimide film, or Polyamide film. 根据权利要求1所述的一种防紫外光夜视兼容薄膜材料,其特征在于:所述防紫外光夜视兼容涂层涂层其原料及各组分质量份如下:紫外吸收剂0.3-0.8质量份,近红外吸收剂0.1~0.5质量份,基体树脂100质量份,树脂固化剂10~25质量份,有机溶剂30~50质量份。The UV-resistant night-vision-compatible film material according to claim 1, wherein the raw materials of the UV-resistant night-vision-compatible coating and the mass fraction of each component are as follows: UV absorber 0.3-0.8 Parts by mass, 0.1 to 0.5 parts by mass of near-infrared absorber, 100 parts by mass of base resin, 10 to 25 parts by mass of resin curing agent, and 30 to 50 parts by mass of organic solvent. 根据权利要求2所述的一种防紫外光夜视兼容薄膜材料,其特征在于:所述紫外吸收剂为苯并三唑UV-360、苯并三唑UV-326或二苯甲酮UV-531。The anti-ultraviolet night vision compatible film material according to claim 2, wherein the ultraviolet absorber is benzotriazole UV-360, benzotriazole UV-326, or benzophenone UV- 531. 根据权利要求2所述的一种防紫外光夜视兼容薄膜材料,其特征在于:所述近红外吸收剂为硫代双烯型镍染料、甲基菁类染料和酞菁类染料中的一种或多种。The anti-ultraviolet night vision compatible film material according to claim 2, wherein the near-infrared absorbing agent is one of a thiodiene-type nickel dye, a methylcyanine dye, and a phthalocyanine dye. Or more. 根据权利要求2所述的一种防紫外光夜视兼容薄膜材料,其特征在于:所述基体树脂为聚甲基丙烯酸甲酯或聚碳酸酯。The anti-ultraviolet night vision compatible film material according to claim 2, wherein the matrix resin is polymethyl methacrylate or polycarbonate. 根据权利要求2所述的一种防紫外光夜视兼容薄膜材料,其特征在于:所述树脂固化剂为脂肪类聚异氰酸酯或脂环类聚异氰酸酯,所述有机溶剂为氯仿、二氯甲烷或丙酮。The anti-ultraviolet night vision compatible film material according to claim 2, wherein the resin curing agent is an aliphatic polyisocyanate or an alicyclic polyisocyanate, and the organic solvent is chloroform, dichloromethane, or acetone. 一种防紫外光夜视兼容薄膜材料的制备方法,其特征在于,其具体步骤如下:A method for preparing a UV-resistant night vision compatible film material is characterized in that the specific steps are as follows: 步骤一,将透明基材表面清洗干净;Step 1: clean the surface of the transparent substrate; 步骤二,按比例称取防紫外光夜视兼容涂层的各原料,溶于有机溶剂中,制得防紫外夜视兼容涂层,将涂层涂覆在步骤一所得透明基材表面;Step 2: Weigh each raw material of the UV-resistant night vision-compatible coating according to the proportion and dissolve it in an organic solvent to prepare a UV-resistant night-vision compatible coating, and apply the coating on the surface of the transparent substrate obtained in step 1. 步骤三,将步骤二中所得薄膜干燥4~6小时,待溶剂挥发后后转移至80℃烘箱固化5~8小时。In step three, the film obtained in step two is dried for 4 to 6 hours. After the solvent is volatilized, it is transferred to an oven at 80 ° C. for curing for 5 to 8 hours.
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