CN112458400B - 一种抗砂尘防潮防霉窗口复合增透膜的制备方法 - Google Patents

一种抗砂尘防潮防霉窗口复合增透膜的制备方法 Download PDF

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CN112458400B
CN112458400B CN202011334442.1A CN202011334442A CN112458400B CN 112458400 B CN112458400 B CN 112458400B CN 202011334442 A CN202011334442 A CN 202011334442A CN 112458400 B CN112458400 B CN 112458400B
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王航
孙义可
熊涛
徐旭
郝博
余雪宁
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Hubei Jiuzhiyang Infrared System Co Ltd
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Abstract

本发明公开了一种抗砂尘防潮防霉窗口复合增透膜的制备方法，对K9基底进行化学钢化，清晰擦拭后装入镀膜夹具放入镀膜机；当本底真空达到1.0×10‑3Pa及以下，同时保证基片250℃恒温至少80分钟后，开启离子源基片表进行离子束刻蚀清洗；由高低折射率膜料SiO2和Ta2O5采用电子束蒸发成膜，并通过离子束辅助沉积；以高纯度HfO2为原料，采用离子辅助沉积工艺，控制沉积速率0.2nm/s；取出镀膜件，涂覆含氟硅的超低表面能丙烯酸树脂溶液吹干。本发明实现了光学窗口表面改性，不仅满足光学增透效果，也使光学窗口薄膜具备了抗砂尘和防霉防潮的功能，同时也能承受住一定的温度冲击。

Description

一种抗砂尘防潮防霉窗口复合增透膜的制备方法
技术领域
本发明属于属于光学薄膜技术领域，具体涉及一种抗砂尘防潮防霉窗口复合增透膜的制备方法。
背景技术
以K9材料为基底的传统窗口广泛应用于海陆空天等各领域光电装备(主要涵盖可见光和近红外波段)，为提高光学窗口的光学性能而在窗口表面镀制的普通增透膜(以SiO2、TiO2、Ta2O5、MgF2等膜层构成)已越来越不适应特殊环境的需求，如：①在一定浓度和颗粒尺寸的砂尘环境下，窗口膜层极易“吹花”，表面光洁度恶化，进而降低光学性能，破坏膜层结构，甚至脱膜。②机载设备光窗在湿度较大或者窗口温度低于大气温度时，窗口表面易挂水珠，影响光学设备成像、探测等多种性能。③光窗长期不进行维护时，表面容易滋生霉菌。④光窗优异的光学性能与耐候性能及机械性能不能兼具。
因此，针对提高光学窗口的机械物理性能的研究一直都在进行中，但是，具有高强硬度保护膜的加入设计，往往由于其相关波段有较大吸收或膜层应力较大等诸多缺点，进而影响到整个光窗的光学性能。鉴于此，亟待在K9基底上开发出一种抗砂尘防潮防霉窗口组合膜系及制备方法，以解决上述问题，并实现工程化应用。
发明内容
本发明目的在于提供一种在K9基片上镀制抗砂尘防潮防霉窗口复合增透膜的制备方法，通过多种膜层的复合重构，大幅提升窗口膜在极端恶劣环境下的使用寿命与维护效率，且工艺重复性好，光学性能优良。
为达到上述目的，采用技术方案如下：
一种抗砂尘防潮防霉窗口复合增透膜的制备方法，包括以下步骤：
1)基片钢化和清洗：对K9基底进行化学钢化，用氧化铈抛光液粗略擦拭一遍，然后用专用无水混合有机溶液精擦，目视检查无残留污染物后装入镀膜夹具，然后放入镀膜机；
2)离子束刻蚀清洗：当本底真空达到1.0×10-3Pa及以下，同时保证基片250℃恒温至少80分钟后，开启离子源基片表进行离子束刻蚀清洗，加速电压1000mA，离子束流700mA，持续4分钟；
3)光学匹配膜系的镀制：由高低折射率膜料SiO2和Ta2O5采用电子束蒸发成膜，并通过离子束辅助沉积；
4)氮氧化铪硬质保护层的镀制：以高纯度HfO2为原料，采用离子辅助沉积工艺，离子源束流增大至1200mA以上，按比例充入工作气体Ar和N2，加热温度升至300℃，控制沉积速率0.2nm/s；
5)表层憎水膜涂覆：待温度降至90℃以下后放气，取出镀膜件，在氮氧化铪硬质保护层上均匀涂覆含氟硅的超低表面能丙烯酸树脂溶液，然后用热风枪吹干。
按上述方案，所述复合增透膜采用Macleod软件进行膜系结构设计：
Sub|aH/bL/cH/dL/eH/fL/gH/hP/Air
其中，H和L分别为高低折射率层，其中H为Ta2O5，L为SiO2；P为硬质保护层HfON，a～h分别为各膜层的物理厚度，依次为：
a-325.8nm；b-424.7nm；c-210.6nm；d-71.6nm；e-434.9nm；f-272.2nm；g-183.7nm；h-610.3nm。
按上述方案，步骤1所述化学钢化过程如下：
将熔盐和待钢化的玻璃在炉内分别以5℃/min速率升温至390℃，将玻璃浸入熔盐恒温30h取出，并以3℃/min速率冷却至常温；熔盐配方为：硝酸钾、氢氧化钾、硅藻土按质量比100:3:8。
按上述方案，步骤3中增加辅助沉积时离子源束流至1000mA以上，同时分别调节SiO2和Ta2O5工艺中Ar和O2流量，Ar流量控制在10sccm，镀制Ta2O5膜层时O2流量60sccm，镀制SiO2膜层时O2流量40sccm。
按上述方案，步骤4中调节工作气体流量N2为40sccm，Ar为10sccm。
本发明相对于现有技术的有益效果在于：通过现有工艺技术，实现了光学窗口表面改性，不仅满足光学增透效果，也使光学窗口薄膜具备了抗砂尘和防霉防潮的功能，同时也能承受住一定的温度冲击，对于军民品光学窗口环境适应性的提升有积极的作用。
附图说明
图1：本发明窗口样件单面镀膜后实测透过率曲线。
具体实施方式
以下实施例进一步阐释本发明的技术方案，但不作为对本发明保护范围的限制。
本发明中一种抗砂尘防潮防霉窗口复合增透膜，K9窗口尺寸174mm×174mm×10mm，具体技术指标如下：
Tavg≥93％@1500-1700nm,AOI＝0-30°
镀膜样片一次性通过GJB2485-95规定的高/低温、恒定湿热，盐雾以及附着力测试与重度摩擦试验，且环境试验前后光学性能仍能满足光学技术指标要求。
通过GJB150.10A/12A中一级霉菌试验和中等浓度砂尘试验。
憎水角度不小于110°。
本发明所涉及的一种抗砂尘防潮防霉K9窗口复合近红外增透膜主要是在新柯隆MIC-1350型真空镀膜机上实现的。该镀膜设备主要配置有NIS-175型大口径射频离子源及中和器、Polycold冷阱、XTC/3S水晶式膜厚仪、上烘烤式加热系统以及OPM-Z1光学式膜厚计等。
首先，根据上述技术要求采用Macleod软件进行膜系结构优化设计，结果如下：
Sub|aH/bL/cH/dL/eH/fL/gH/hP/Air
其中，H和L分别为高低折射率层，其中H为Ta2O5，L为SiO2；P为硬质保护层HfON，a～h分别为各膜层的物理厚度，依次为：
a-325.8nm；b-424.7nm；c-210.6nm；d-71.6nm；e-434.9nm；f-272.2nm；g-183.7nm；h-610.3nm。
制备过程具体实施过程如下：
基片准备：首先对K9基片进行化学钢化，再在镀膜前对基底用氧化铈抛光液粗略擦拭一遍，然后用专用无水混合有机溶液精擦，目视检查无残留污染物后装入专用镀膜夹具，然后放入镀膜机；
化学钢化过程如下：将熔盐和待钢化的玻璃在炉内分别以5℃/min速率升温至390℃，将玻璃浸入熔盐恒温30h取出，并以3℃/min速率冷却至常温；熔盐配方为：硝酸钾、氢氧化钾、硅藻土按质量比100:3:8。
离子束刻蚀清洗：待本底真空达到1.0×10-3Pa及以下，同时保证基片250℃恒温至少80分钟后，开启离子源基片表进行离子束刻蚀清洗，氩气20sccm，氧气20sccm，离子束流700mA，持续4分钟。
在基片上蒸镀光学多层匹配膜系：沉积温度250℃，增加辅助沉积时离子源束流1000mA，同时调节离子源工作气体流量——Ta2O5时O2流量60sccm，SiO2时O2流量40sccm。
在光学多层匹配膜系上镀制高硬度氮氧化铪硬质保护层：注意和匹配膜系镀制过程衔接，加热温度升至300℃，恒温20分钟后开始镀膜，控制沉积速率0.2nm/s。离子源束流增大至1200mA以上，按比例充入工作气体Ar(10sccm)和N2(50sccm)。
镀膜结束后，待温度降至90℃以下后放气，取出镀膜件。用棉球蘸取含氟硅的超低表面能丙烯酸树脂溶液，在高硬度氮氧化铪硬质保护层上均匀涂覆，同时用热风枪调温至80℃吹干。
实施例所得抗砂尘防潮防霉窗口复合增透膜通过了GJB150.12A中等浓度(1.1g/cm3±0.3g/cm3)砂尘试验和GJB150.10A的一级霉菌试验，样品在水滴测角仪上测量得出水滴的接触角为114.6°，具备较好的憎水(防潮)效果。另外还具备较好的抗温度冲击能力，已经过如下试验：窗口样品加热至55℃，迅速放入-5℃的冷水中，窗口完好无损。
图1为本实施例所得窗口样件单面镀膜后实测透过率曲线，经计算1500-1700nm平均透过率约为94.2％。

Claims (3)

1.一种抗砂尘防潮防霉窗口复合增透膜的制备方法，其特征在于包括以下步骤：
1)基片钢化和清洗：对K9基底进行化学钢化，用氧化铈抛光液粗略擦拭一遍，然后用专用无水混合有机溶液精擦，目视检查无残留污染物后装入镀膜夹具，然后放入镀膜机；
2)离子束刻蚀清洗：当本底真空达到1.0×10-3Pa及以下，同时保证基片250℃恒温至少80分钟后，开启离子源基片表进行离子束刻蚀清洗，加速电压1000mA，离子束流700mA，持续4分钟；
3)光学匹配膜系的镀制：由高低折射率膜料SiO2和Ta2O5采用电子束蒸发成膜，并通过离子束辅助沉积；
4)氮氧化铪硬质保护层的镀制：以高纯度HfO2为原料，采用离子辅助沉积工艺，离子源束流增大至1200mA以上，按比例充入工作气体Ar和N2，加热温度升至300℃，控制沉积速率0.2nm/s；工作气体流量N2为40sccm，Ar为10sccm；
5)表层憎水膜涂覆：待温度降至90℃以下后放气，取出镀膜件，在氮氧化铪硬质保护层上均匀涂覆含氟硅的超低表面能丙烯酸树脂溶液，然后用热风枪吹干；
所述复合增透膜采用Macleod软件进行膜系结构设计：
Sub|aH/bL/cH/dL/eH/fL/gH/hP/Air
其中，H和L分别为高低折射率层，其中H为Ta2O5，L为SiO2；P为硬质保护层HfON，a～h分别为各膜层的物理厚度，依次为：
a-325.8nm；b-424.7nm；c-210.6nm；d-71.6nm；e-434.9nm；f-272.2nm；g-183.7nm；h-610.3nm。
2.如权利要求1所述抗砂尘防潮防霉窗口复合增透膜的制备方法，其特征在于步骤1所述化学钢化过程如下：
将熔盐和待钢化的玻璃在炉内分别以5℃/min速率升温至390℃，将玻璃浸入熔盐恒温30h取出，并以3℃/min速率冷却至常温；熔盐配方为：硝酸钾、氢氧化钾、硅藻土按质量比100:3:8。
3.如权利要求1所述抗砂尘防潮防霉窗口复合增透膜的制备方法，其特征在于步骤3中增加辅助沉积时离子源束流至1000mA以上，同时分别调节SiO2和Ta2O5工艺中Ar和O2流量，Ar流量控制在10sccm，镀制Ta2O5膜层时O2流量60sccm，镀制SiO2膜层时O2流量40sccm。
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