CN116083866A - 一种3d车载玻璃表面镀膜工艺 - Google Patents
一种3d车载玻璃表面镀膜工艺 Download PDFInfo
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Abstract
本发明公开了一种3D车载玻璃表面镀膜工艺，属于车载玻璃技术领域，包括玻璃基面预处理、抽真空、预溅射和溅射镀膜过程，溅射镀膜过程中在3D车载玻璃的镀膜基面上，从里到外依次镀设高折射率层、低折射率层和抗指纹层，本发明通过高折射率层和低折射率层交替设置形成了耐光学反射层，耐光学反射层能够有效减少外部光线在3D车载玻璃表面的反射光；在进行抗指纹层的镀设过程中，采用了钛和聚四氟乙烯作为混合靶材，同时采用了氮气和氩气作为溅射气氛进行磁控溅射，在3D车载玻璃表面形成氮化钛和聚四氟乙烯的抗指纹镀层，该抗指纹镀层具有较好的抗水抗油特性，能够有效避免指纹对3D车载玻璃表面的污染。
Description
技术领域
本发明属于车载玻璃技术领域，具体涉及一种3D车载玻璃表面镀膜工艺。
背景技术
随着汽车电动化、智能化、互联网化等趋势日益在汽车市场渗透发展，中高档汽车触摸屏对3D车载玻璃的需求日益快速增长，3D车载玻璃正在成为车载玻璃市场的蓝海。
3D车载玻璃的生产工序包括开料-CNC1(玻璃铣削)-热弯-CNC2-抛光-丝印/黄光-镀膜-包装。其中，镀膜工艺是3D车载玻璃制造中的重点工序，3D车载玻璃表面需要镀设AR镀膜(减光学反射镀膜)和AF镀膜(抗指纹镀膜)，玻璃表面镀膜技术包括溶胶-凝胶覆膜、磁控溅射镀膜、化学气相沉积镀膜。
现有的AR镀膜工艺中，一般采用辊涂镀膜工艺或者采用化学气相沉积镀膜工艺，制备的AR镀膜玻璃通过多孔S iO2溶胶成膜，膜层显示深蓝紫色，中国专利CN101885586B公开一种光伏玻璃表面减反射膜的制备方法，包括如下步骤：制备无机-有机杂化硅溶胶：涂膜：疏水处理：固化处理。其优点在于：减反射膜与衬底光伏玻璃之间的膜基结合力较强，从而提高了镀膜光伏玻璃表面减反膜的耐擦拭性能。溶胶凝胶法制备减反膜尽管生产成本较低，但工艺稳定性不足，控制难度很大。
发明内容
本发明的目的在于提供一种3D车载玻璃表面镀膜工艺，本发明拟采用磁控溅射镀膜工艺，磁控溅射镀膜是利用荷能粒子去轰击靶材，把部分能量传给靶材原子，靶材原子从靶材中溅射出来在基体表面沉积，并形成薄膜。磁控溅射镀膜分为直流磁控溅射、中频磁控溅射、射频磁控溅射。磁控溅射镀膜玻璃常用于高端领域，除了电致变色膜，还可用于制备光热控制膜、增透减反射膜等常见玻璃表面功能膜。本发明旨在通过改进磁控溅射镀膜工艺，提供一种3D车载玻璃表面AR镀膜和AF镀膜的整体镀设工艺，最终得到一种耐光学反射和抗指纹性能俱佳的3D车载玻璃，以解决背景技术中的问题。
本发明的目的可以通过以下技术方案实现：
一种3D车载玻璃表面镀膜工艺，包括以下步骤：
S1、抽真空：将3D车载玻璃置于磁控溅射沉积***的镀膜室的溅射样品台上，将镀膜室内的真空度调整至0.0035-0.005Pa；
S2、预溅射：在室温条件下，调控磁控溅射沉积***的靶基距为70-80mm，溅射气氛为高纯度的保护气，溅射气压为1.2-1.4Pa，靶功率为85-110W，溅射时间为5-8min，完成3D车载玻璃的预溅射；
S3、溅射镀膜：在3D车载玻璃的镀膜基面上，从里到外依次镀设高折射率层、低折射率层和抗指纹层，调控溅射气压为1.0-1.2Pa，靶功率为70-95W，溅射时间为55-85min，溅射完成后，冷却至室温，得复合层镀膜玻璃，完成3D车载玻璃的表面镀膜工艺。
进一步地，所述保护气为氩气或氮气。
进一步地，所述高折射率层的靶材为TiO2、Nb2O5和ZrO中的一种，所述高折射率层的镀膜厚度为30nm-75nm。
进一步地，所述低折射率层的靶材为SiO2和AlF3中的一种，所述低折射率层的镀膜厚度为35nm-90nm。
进一步地，所述抗指纹层的靶材为混合靶材，所述混合靶材的制备过程：将钛粉和聚四氟乙烯微粉按照质量比1.25-1.3：1充分搅拌混合后压块，得所述混合靶材。
进一步地，所述抗指纹层的镀膜厚度为45nm-150nm。
进一步地，所述3D车载玻璃在镀膜前需经预处理：利用无水乙醇对3D车载玻璃的镀膜基面进行超声清洗15min，接着用去离子水超声清洗15min，再置于80℃条件的烘干室内干燥30min，完成3D车载玻璃的预处理。
本发明的有益效果：
本发明提供的一种3D车载玻璃表面镀膜工艺，通过高折射率层和低折射率层交替层形成了耐光学反射层，通过所述耐光学反射层能够有效减少外部光线在3D车载玻璃表面的反射光；在进行抗指纹层的镀设过程中，采用了钛和聚四氟乙烯作为混合靶材，同时采用了氮气和氩气作为溅射气氛进行磁控溅射，在3D车载玻璃表面形成氮化钛和聚四氟乙烯的抗指纹镀层，该抗指纹镀层具有较好的抗水抗油特性，能够有效避免指纹对3D车载玻璃表面的污染。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
靶材的制备和选择：
高折射率层的靶材为TiO2；
低折射率层的靶材为SiO2；
抗指纹层的靶材为混合靶材，所述混合靶材的制备过程：将钛粉和聚四氟乙烯微粉按照质量比1.25：1充分搅拌混合后压块。
实施例2
靶材的制备和选择：
高折射率层的靶材为Nb2O5；
低折射率层的靶材为SiO2；
抗指纹层的靶材为混合靶材，所述混合靶材的制备过程：将钛粉和聚四氟乙烯微粉按照质量比1.25：1充分搅拌混合后压块。
实施例3
靶材的制备和选择：
高折射率层的靶材为ZrO；
低折射率层的靶材为AlF3；
抗指纹层的靶材为混合靶材，所述混合靶材的制备过程：将钛粉和聚四氟乙烯微粉按照质量比1.3：1充分搅拌混合后压块。
实施例4
一种3D车载玻璃表面镀膜工艺，包括以下步骤：
S1、预处理：利用无水乙醇对3D车载玻璃的镀膜基面进行超声清洗15min，接着用去离子水超声清洗15min，再置于80℃条件的烘干室内干燥30min，完成3D车载玻璃的预处理；
S2、抽真空：将3D车载玻璃置于磁控溅射沉积***的镀膜室的溅射样品台上，将镀膜室内的真空度调整至0.0035Pa；
S3、预溅射：在室温条件下，调控磁控溅射沉积***的靶基距为70mm，溅射气氛为高纯度的氩气，溅射气压为1.2Pa，靶功率为85W，溅射时间为5min，完成3D车载玻璃的预溅射；
S4、溅射镀膜：在3D车载玻璃的镀膜基面上，从里到外依次镀设30nm的高折射率层、35nm的低折射率层和45nm的抗指纹层，相应层的靶材原料依据实施例1确实，调控溅射气压为1.0Pa，靶功率为70W，溅射时间为55min，溅射完成后，冷却至室温，得复合层镀膜玻璃，完成3D车载玻璃的表面镀膜工艺。
实施例5
一种3D车载玻璃表面镀膜工艺，包括以下步骤：
S1、预处理：利用无水乙醇对3D车载玻璃的镀膜基面进行超声清洗15min，接着用去离子水超声清洗15min，再置于80℃条件的烘干室内干燥30min，完成3D车载玻璃的预处理；
S2、抽真空：将3D车载玻璃置于磁控溅射沉积***的镀膜室的溅射样品台上，将镀膜室内的真空度调整至0.0045Pa；
S3、预溅射：在室温条件下，调控磁控溅射沉积***的靶基距为75mm，溅射气氛为高纯度的氮气，溅射气压为1.3Pa，靶功率为95W，溅射时间为7min，完成3D车载玻璃的预溅射；
S4、溅射镀膜：在3D车载玻璃的镀膜基面上，从里到外依次镀设65nm的高折射率层、45nm的低折射率层和85nm的抗指纹层，相应层的靶材原料依据实施例2确实，调控溅射气压为1.1Pa，靶功率为80W，溅射时间为75min，溅射完成后，冷却至室温，得复合层镀膜玻璃，完成3D车载玻璃的表面镀膜工艺。
实施例6
一种3D车载玻璃表面镀膜工艺，包括以下步骤：
S1、预处理：利用无水乙醇对3D车载玻璃的镀膜基面进行超声清洗15min，接着用去离子水超声清洗15min，再置于80℃条件的烘干室内干燥30min，完成3D车载玻璃的预处理；
S2、抽真空：将3D车载玻璃置于磁控溅射沉积***的镀膜室的溅射样品台上，将镀膜室内的真空度调整至0.005Pa；
S3、预溅射：在室温条件下，调控磁控溅射沉积***的靶基距为80mm，溅射气氛为高纯度的氮气，溅射气压为1.4Pa，靶功率为110W，溅射时间为8min，完成3D车载玻璃的预溅射；
S4、溅射镀膜：在3D车载玻璃的镀膜基面上，从里到外依次镀设75nm的高折射率层、90nm的低折射率层和150nm的抗指纹层，相应层的靶材原料依据实施例3确实，调控溅射气压为1.2Pa，靶功率为95W，溅射时间为85min，溅射完成后，冷却至室温，得复合层镀膜玻璃，完成3D车载玻璃的表面镀膜工艺。
对实施例4-实施例6制备的表面镀膜的3D车载玻璃进行性能测试，检测过程如下，检测结果如表1所示：
反射率测试：按照GBT2680-1994公开的太阳光各波段分布特性，测试各实施例和对比例样品的反射率；
抗指纹性能测试：采用SITA表面清洁度仪测定镀膜前后的3D车载玻璃表面清洁度，主要通过检测出油脂、指印等污染物，表征3D车载玻璃的抗指纹性能，SITA表面清洁度仪以RFU值(Relative Fluorescence Units)表示清洁度的高度，RFU为相对荧光强度值，RFU值越大，3D车载玻璃表面污染物含量越高，具体检测过程如下：
玻璃样品包括实施例4-实施例6制备的表面镀膜的3D车载玻璃和未经镀膜的3D车载玻璃，样品共六组，每组设置三个玻璃单样，在每个玻璃单样表面选取十个测试点，用手指指压测试点，通过仪器检测每组玻璃单样每个测试点的RFU值，仪器自动计算出平均值。
表1
由表1可以看出，采用本发明提供的3D车载玻璃表面镀膜工艺制备得到的3D车载玻璃表面的镀膜结构具有较低的反射率和RFU值，本发明提供了一种耐光学反射和抗指纹性能俱佳的3D车载玻璃的镀膜工艺。
需要说明的是，在本文中，诸如术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。
Claims (7)
1.一种3D车载玻璃表面镀膜工艺，其特征在于，包括以下步骤：
S1、抽真空：将3D车载玻璃置于磁控溅射沉积***的镀膜室的溅射样品台上，将镀膜室内的真空度调整至0.0035-0.005Pa；
S2、预溅射：在室温条件下，调控磁控溅射沉积***的靶基距为70-80mm，溅射气氛为高纯度的保护气，溅射气压为1.2-1.4Pa，靶功率为85-110W，溅射时间为5-8min，完成3D车载玻璃的预溅射；
S3、溅射镀膜：在3D车载玻璃的镀膜基面上，从里到外依次镀设高折射率层、低折射率层和抗指纹层，调控溅射气压为1.0-1.2Pa，靶功率为70-95W，溅射时间为55-85min，溅射完成后，冷却至室温，得复合层镀膜玻璃，完成3D车载玻璃的表面镀膜工艺。
2.根据权利要求1所述的一种3D车载玻璃表面镀膜工艺，其特征在于，所述保护气为氩气或氮气。
3.根据权利要求1所述的一种3D车载玻璃表面镀膜工艺，其特征在于，所述高折射率层的靶材为TiO2、Nb2O5和ZrO中的一种，所述高折射率层的镀膜厚度为30nm-75nm。
4.根据权利要求1所述的一种3D车载玻璃表面镀膜工艺，其特征在于，所述低折射率层的靶材为SiO2和AlF3中的一种，所述低折射率层的镀膜厚度为35nm-90nm。
5.根据权利要求1所述的一种3D车载玻璃表面镀膜工艺，其特征在于，所述抗指纹层的靶材为混合靶材，所述混合靶材的制备过程：将钛粉和聚四氟乙烯微粉按照质量比1.25-1.3：1充分搅拌混合后压块，得所述混合靶材。
6.根据权利要求1所述的一种3D车载玻璃表面镀膜工艺，其特征在于，所述抗指纹层的镀膜厚度为45nm-150nm。
7.根据权利要求1所述的一种3D车载玻璃表面镀膜工艺，其特征在于，所述3D车载玻璃在镀膜前需经预处理：利用无水乙醇对3D车载玻璃的镀膜基面进行超声清洗15min，接着用去离子水超声清洗15min，再置于80℃条件的烘干室内干燥30min，完成3D车载玻璃的预处理。
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| US20040071889A1 (en) * | 2002-08-07 | 2004-04-15 | Hoya Corporation | Method of producing an antireflection-coated substrate |
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| CN111826622A (zh) * | 2020-06-10 | 2020-10-27 | 深圳市锐欧光学电子有限公司 | 一种手机摄像头盖板镀膜方法 |
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| US20040071889A1 (en) * | 2002-08-07 | 2004-04-15 | Hoya Corporation | Method of producing an antireflection-coated substrate |
| CN108441837A (zh) * | 2018-06-13 | 2018-08-24 | 天津南玻节能玻璃有限公司 | 一种减反射镀膜结构 |
| CN111153601A (zh) * | 2020-01-16 | 2020-05-15 | 苏州胜利精密制造科技股份有限公司 | 减反射曲面玻璃盖板及制备方法 |
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