CN106045333B - 一种低辐射镀膜玻璃及其制备方法 - Google Patents

一种低辐射镀膜玻璃及其制备方法 Download PDF

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CN106045333B
CN106045333B CN201610653469.4A CN201610653469A CN106045333B CN 106045333 B CN106045333 B CN 106045333B CN 201610653469 A CN201610653469 A CN 201610653469A CN 106045333 B CN106045333 B CN 106045333B
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时方晓
仝玉莲
高旭
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Yaohua Qinhuangdao Glass Co ltd
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3647—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer in combination with other metals, silver being more than 50%
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
    • C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
    • C03C17/3657—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the multilayer coating having optical properties
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    • C03C2218/00—Methods for coating glass
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    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering
    • C03C2218/156—Deposition methods from the vapour phase by sputtering by magnetron sputtering

Abstract

本发明提供一种低辐射镀膜玻璃及其制备方法，所述低辐射镀膜玻璃包括玻璃基片及依次溅射于玻璃基片之上的内层介质层、功能层和外层介质层；所述内层介质层和外层介质层均为(Ti,Al)N薄膜，功能层为掺铜银膜，并且在功能层和外层介质层之间还可溅射一层防氧化层。所述制备方法包括：将玻璃基片于氩气和氮气氛围中溅射内层介质层；然后于氩气氛围中在内层介质层上溅射功能层；再于氩气和氮气氛围中在功能层上溅射外层介质层，得到低辐射镀膜玻璃。本发明的低辐射镀膜玻璃的辐射率为0.052~0.054，光透过率为74.4~78.36%，远红外反射率为99.8~99.99%。

Description

一种低辐射镀膜玻璃及其制备方法
技术领域
本发明涉及镀膜玻璃技术领域，具体涉及一种低辐射镀膜玻璃及其制备方法。
背景技术
低辐射镀膜玻璃是在玻璃表面上沉积多层膜物质，使其具有高可见光透过率和高远红外反射率，从而达到保温隔热的目的，其广泛应用于建筑及其它行业，常用来做玻璃幕墙结构、门窗、车窗等等，以减少空调能耗，达到节能环保的目的。
目前，市售的普通低辐射镀膜玻璃的光学性能较差，可见光透过率低于80%，红外反射率只有70%左右。并且它们大多采用纯银功能层，由于银极易被氧化，会较快失去作用，从而使低辐射镀膜玻璃丧失保温隔热的功能，且银的耐候性较差，潮湿环境下空气中的水蒸汽通过扩散进入银层使膜中的银原子发生迁移聚集，从而造成在银层上沉积的介质层的应力过大而发生脱膜形成白点，造成镀膜玻璃的报废。目前关于低辐射镀膜玻璃银层掺杂性能的工艺研究备受关注，但大多效果不尽如人意。因此开发一种具有优异光学性能的低辐射镀膜玻璃及其制备方法具有重要意义。
发明内容
本发明的目的在于改善当前低辐射镀膜玻璃的缺陷，优化其性能，提供一种高远红外反射率、性能稳定的低辐射镀膜玻璃及其制备方法。本发明的技术方案为：
一种低辐射镀膜玻璃，包括玻璃基片及依次溅射于玻璃基片之上的内层介质层、功能层和外层介质层；所述内层介质层和外层介质层均为(Ti,Al)N薄膜，功能层为掺铜银膜。
所述内层介质层和外层介质层中铝含量分别为0.66±0.1%、0.36±0.1%，膜层厚度分别为200~210nm和140~160nm，内层介质层的作用在于增强功能膜与玻璃基底的附着力，同时可调节膜系的光学性能和颜色，外层介质层的作用为保护功能层，防止其被氧化，亦是减反膜，在可见光和近红外太阳能光谱中起减反作用，以提高波长范围内的太阳能透射比，提高膜系物理化学性能。
所述功能层中银铜的质量配比为2:1，膜层厚度为90~100nm，该层的作用为产生低辐射效果，铜银合金层太阳能反射率较高，机械性能、硬度及耐温性能好。
为使镀膜玻璃膜层结构获得更优越的稳定性和耐久性，还可以在上述功能层和外层介质层之间溅射一层防氧化层，所述防氧化层为钛薄膜，膜层厚度为10~20nm。
所述低辐射镀膜玻璃的制备方法，包括：
（1）将玻璃基片洗净干燥；
（2）于氩气和氮气氛围中在玻璃基片上溅射内层介质层，溅射条件为：真空度为3×10-3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为80~85W和90~100W，溅射时间为90min；
（3）于氩气氛围中在内层介质层上溅射功能层，溅射条件为：真空度为3×10-3Pa，Ag靶和Cu靶的功率均为96W，溅射时间为5s，溅射完毕使功能层隔绝空气；
（4）于氩气和氮气氛围中在功能层上溅射外层介质层，溅射条件为：真空度为3×10-3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为70~75W和60~65W，溅射时间为40min，得到低辐射镀膜玻璃。
所述低辐射镀膜玻璃的辐射率为0.052~0.054，光透过率为74.4~78.36%，远红外反射率为99.8~99.99%。
本发明的有益效果为：本发明采用银铜质量配比为2:1的掺铜银膜作为功能层，在降低镀膜玻璃辐射率的同时提高其光透射率和远红外反射率，本发明的低辐射镀膜玻璃的辐射率为0.052~0.054，光透过率为74.4~78.36%，远红外反射率为99.8~99.99%，而现有的市售单银低辐射镀膜玻璃的辐射率为0.1左右，光透过率最高达到约70%，远红外反射率只有70%左右。同时，本发明为优化制备工艺，还提出在功能层和外层介质层之间增加溅射一层防氧化层以解决换靶时易氧化的问题。此外，本发明采用溅射镀膜法在玻璃基片上制备薄膜，膜基结合力较强，使用寿命较长，膜的均匀性较好且性能较稳定。
附图说明
图1为本发明实施例1所制备的低辐射镀膜玻璃的结构示意图；
图2为本发明实施例2所制备的低辐射镀膜玻璃的结构示意图；
其中：1—玻璃基片；2—内层介质层（(Ti,Al)N）；3—功能层（掺铜银膜）；4—外层介质层（(Ti,Al)N）；5—过渡层（Ti）。
具体实施方式
以下通过具体实施例结合附图对本发明的具体实施过程进行叙述，但实施例的内容并不限制本发明的保护范围。
实施例1
一种低辐射镀膜玻璃，其结构如图1所示，包括钠钙玻璃基片及依次溅射于钠钙玻璃基片之上的内层(Ti,Al)N薄膜层、掺铜银膜层和外层(Ti,Al)N薄膜层；其中钠钙玻璃基片厚度为1mm；内层(Ti,Al)N薄膜层和外层(Ti,Al)N薄膜层中铝含量分别为0.66±0.1%、0.36±0.1%，膜层厚度分别为206nm和150nm；掺铜银膜层中银铜的质量配比为2:1，膜层厚度为90nm。
所述低辐射镀膜玻璃的制备方法，采用磁控溅射技术，包括：
（1）将钠钙玻璃基片经标准化学清洗程序清洗干净，然后用蘸有无水乙醇的脱脂棉擦拭干净，放入装有无水乙醇的烧杯中超声波清洗15min，取出置于装有去离子水的烧杯中超声波清洗10min，取出并经氮气吹干后置于干燥箱中备用；
（2）将钠钙玻璃基片放入磁控溅射镀膜机真空室内可随转台转动的样品托架上，设定转动样品托架的转速为80%，以纯度为99.99%的氩气为离化气体，纯度为99.99%的氮气为反应气体，在钠钙玻璃基片上溅射内层(Ti,Al)N薄膜层，溅射条件为：真空度为3×10- 3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为80~85W和90~100W，溅射时间为90min；
（3）于氩气氛围中在内层(Ti,Al)N薄膜层上溅射掺铜银膜层，溅射条件为：真空度为3×10-3Pa，Ag靶和Cu靶的功率均为96W，溅射时间为5s，溅射完毕使镀膜的钠钙玻璃基片隔绝空气以防掺铜银膜层被氧化；
（4）于氩气和氮气氛围中在掺铜银膜层上溅射外层(Ti,Al)N薄膜层，溅射条件为：真空度为3×10-3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为70~75W和60~65W，溅射时间为40min，得到低辐射镀膜玻璃。
所述低辐射镀膜玻璃的辐射率为0.052，光透过率为74.4%，远红外反射率为99.8%。
实施例2
本实施例的低辐射镀膜玻璃的结构与实施例1相似，如图2所示，与实施例1的区别点在于：玻璃基片为单晶硅片，并且为使镀膜玻璃膜层结构获得更优越的稳定性和耐久性，在功能层和外层介质层之间溅射一层钛薄膜防氧化层，并且钛薄膜厚度为20nm。
所述低辐射镀膜玻璃的制备方法，采用磁控溅射技术，包括：
（1）将单晶硅片经标准化学清洗程序清洗干净，然后用蘸有无水乙醇的脱脂棉擦拭干净，放入装有无水乙醇的烧杯中超声波清洗15min，取出置于装有去离子水的烧杯中超声波清洗10min，取出并经氮气吹干后置于干燥箱中备用；
（2）将单晶硅片放入磁控溅射镀膜机真空室内可随转台转动的样品托架上，设定转动样品托架的转速为80%，以纯度为99.99%的氩气为离化气体，纯度为99.99%的氮气为反应气体，在钠钙玻璃基片上溅射内层(Ti,Al)N薄膜层，溅射条件为：真空度为3×10-3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为80~85W和90~100W，溅射时间为90min；
（3）于氩气氛围中在内层(Ti,Al)N薄膜层上溅射掺铜银膜层，溅射条件为：真空度为3×10-3Pa，Ag靶和Cu靶的功率均为96W，溅射时间为5s，溅射完毕使镀膜的钠钙玻璃基片隔绝空气以防掺铜银膜层被氧化；
（4）于氩气氛围中在掺铜银膜层上溅射Ti膜层，溅射条件为：真空度为3×10-3Pa，Ti靶的功率取起辉功率，溅射时间为10min；
（5）于氩气和氮气氛围中在掺铜银膜层上溅射外层(Ti,Al)N薄膜层，溅射条件为：真空度为3×10-3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为70~75W和60~65W，溅射时间为40min，得到低辐射镀膜玻璃。
所述低辐射镀膜玻璃的辐射率为0.054，光透过率为78.36%，远红外反射率为99.99%。

Claims (4)

1.一种低辐射镀膜玻璃，包括玻璃基片及依次溅射于玻璃基片之上的内层介质层、功能层和外层介质层；其特征在于所述内层介质层和外层介质层均为(Ti,Al)N薄膜，功能层为掺铜银膜；所述内层介质层和所述外层介质层中铝含量分别为0.56~0.76%、0.26~0.46%，膜层厚度分别为200~210nm和140~160nm；所述功能层中银铜的质量配比为2:1，膜层厚度为90~100nm。
2.一种低辐射镀膜玻璃，包括玻璃基片及依次溅射于玻璃基片之上的内层介质层、功能层和外层介质层；其特征在于所述功能层和外层介质层之间还有一层防氧化层，所述防氧化层为钛薄膜，膜层厚度为10~20nm；所述内层介质层和外层介质层均为(Ti,Al)N薄膜，所述内层介质层和所述外层介质层中铝含量分别为0.56~0.76%、0.26~0.46%，膜层厚度分别为200~210nm和140~160nm；功能层为掺铜银膜，所述功能层中银铜的质量配比为2:1，膜层厚度为90~100nm。
3.根据权利要求1或2所述的一种低辐射镀膜玻璃，其特征在于所述低辐射镀膜玻璃的辐射率为0.052~0.054，光透过率为74.4~78.36%，远红外反射率为99.8~99.99%。
4.权利要求1所述的一种低辐射镀膜玻璃的制备方法，其特征在于工艺步骤包括：
（1）将厚度为1mm的玻璃基片洗净干燥；
（2）于氩气和氮气氛围中在玻璃基片上溅射内层介质层，溅射条件为：真空度为3×10- 3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为80~85W和90~100W，溅射时间为90min；
（3）于氩气氛围中在内层介质层上溅射功能层，溅射条件为：真空度为3×10-3Pa，Ag靶和Cu靶的功率均为96W，溅射时间为5s，溅射完毕使功能层隔绝空气；
（4）于氩气和氮气氛围中在功能层上溅射外层介质层，溅射条件为：真空度为3×10- 3Pa，氮气和氩气的体积比为（1~2）:5，Ti靶和Al靶的功率分别为70~75W和60~65W，溅射时间为40min，得到低辐射镀膜玻璃。
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