CN107526120B - 一种镀金刚膜的红外硫系玻璃镜片及其制备方法 - Google Patents
一种镀金刚膜的红外硫系玻璃镜片及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种镀金刚膜的红外硫系玻璃镜片及其制备方法。一种镀金刚膜的红外硫系玻璃镜片,其红外硫系玻璃镜片的表面由内至外依次设置第一Ge膜层、第一ZnSe膜层、第二Ge膜层、第二ZnSe膜层、YF3膜层和AlSi膜层。同时也公开了这种镀金刚膜的红外硫系玻璃镜片的制备方法。本发明根据红外镜片光学薄膜光谱透过规格要求设计特殊膜系,使用特殊膜料不同膜厚度搭配及镀膜机台设定特殊条件下进行蒸镀制备红外硫系玻璃镜片,不但实现了红外镜片光学薄膜光谱透过规格要求,还一次实现得到红外镜片耐磨擦的光学薄膜金刚膜层,且每次蒸镀光学薄膜光谱透过率及薄膜厚度都有很好的再现性,保证了膜的质量及光学光谱稳定。
Description
技术领域
本发明涉及一种镀金刚膜的红外硫系玻璃镜片及其制备方法。
背景技术
远红外玻璃是以Ge、As、Se、Sb为主要元素所形成材料玻璃(又称为硫系玻璃),其是一种非氧化物玻璃。由于硫系玻璃特殊的结构及组分在2~14μm之间具有良好的透过率、极低的折射率温度热系数和色散性、易制备等优点,因此硫系玻璃是一种在红外应用上很广的红外光学玻璃,已用于军用光学系统中、红外热像仪光学镜头、导航仪、民用车载夜视等相关领域。
现在的应用存在如下的问题:镜头的第一片镜片窗口片在日常使用中均会与灰尘或风砂粒等进行玻璃表面磨擦产生粗细不均划伤、划痕;粗细不均的划伤、划痕直接影响到镜头的外观美观度和窗口片的强度,也会造成红外镜片光学透过率降低。针对以上问题,如果是普通氧化物玻璃的话,在玻璃表面加镀一层氧化铝膜就可以增加玻璃表面的硬度起到保护镜片玻璃表面的作用;镀氧化铝后普通玻璃在可见光范围内透过率不会因吸收损失很大;氧化物玻璃材质硬度高,在外力作用下也不易产生破裂或伤痕;且氧化物玻璃在光学薄膜蒸镀中,受到应力影响较小容易实现优质光谱需求光学薄膜。
对于红外镜片硫系玻璃,其在特质上又与其它普通氧化物玻璃的特质不同。红外镜片硫系玻璃材质较软和脆,极容易受外力损伤和破裂。如使用现有技术方法直接镀制一层氧化铝会产生以下多种影响红外镜片性能的不良缺点:1)采用现有技术在硫系玻璃表面镀一层氧化铝膜,不但未能满足红外光学薄膜光谱需求规格透过率,也会因氧化铝的光学特性在0.14~6μm波长透过,在6μm以后透过则是吸收,致远红外长波6~14μm透过率被吸收掉,达不到所需求红外8~12μm透过率Tave≥95%的要求;2)红外镜片硫系玻璃材质较软和脆,极容易受外力损伤和破裂;依现有技术在玻璃窗口片表面镀一层150nm左右厚度氧化铝膜,并不能真正起到保护窗口片基板作用,窗口片与风砂接触表面极容易产生与灰尘、风砂磨擦划伤或受力破损;3)红外硫系玻璃在光学薄膜蒸镀中,会受应力影响较大薄膜附着力差;依现有技术镀制保护膜层易产生膜脱、龟裂、抗耐磨擦性弱,特别使用3M胶带作拉力测试容易膜脱掉膜。
现有技术不能实现对红外镜片红外光学薄膜光谱规格要求及对窗口片真正保护,所以目前亟需研发一种满足红外光学薄膜光谱透过规格要求,光谱透过率及薄膜厚度再现性好的红外硫系玻璃镜片制备方法。
发明内容
本发明的目的在于提供一种镀金刚膜的红外硫系玻璃镜片及其制备方法。
本发明所采取的技术方案是:
一种镀金刚膜的红外硫系玻璃镜片,其红外硫系玻璃镜片的表面由内至外依次设置第一Ge膜层、第一ZnSe膜层、第二Ge膜层、第二ZnSe膜层、YF3膜层和AlSi膜层。
第一Ge膜层的厚度为215~225nm,第一ZnSe膜层的厚度为460~470nm,第二Ge膜层的厚度为230~240nm、第二ZnSe膜层的厚度为420~430nm、YF3膜层的厚度为1220~1240nm,AlSi膜层的厚度为230~240nm。
一种镀金刚膜的红外硫系玻璃镜片的制备方法,是将待镀膜的红外硫系玻璃镜片清洗,烘烤后,依次在镜片表面蒸镀第一Ge膜、第一ZnSe膜、第二Ge膜、第二ZnSe膜、YF3膜和AlSi膜,然后再烘烤制成。
制备方法中,蒸镀AlSi膜所用的膜料为Al2O3和SiO2组成的AlSi混合物。
AlSi混合物在550nm下的折射率为1.46~1.50。
制备方法中,清洗为离子清洗机清洗。
制备方法中,离子清洗机的离子源为氩气。
制备方法中,清洗的时间为15~50min。
制备方法中,蒸镀前,烘烤的温度为80~180℃,烘烤的时间为50~120min。
制备方法中,蒸镀后,烘烤的温度为80~120℃,烘烤的时间为50~150min。
本发明的有益效果是:
本发明根据红外镜片光学薄膜光谱透过规格要求设计特殊膜系,使用特殊膜料不同膜厚度搭配及镀膜机台设定特殊条件下进行蒸镀制备红外硫系玻璃镜片,不但实现了红外镜片光学薄膜光谱透过规格要求,还一次实现得到红外镜片耐磨擦的光学薄膜金刚膜层,且每次蒸镀光学薄膜光谱透过率及薄膜厚度都有很好的再现性,保证了膜的质量及光学光谱稳定。
附图说明
图1是本发明镀金刚膜红外硫系玻璃镜片的结构示意图;
图2是本发明对比例1的硫系玻璃镜片红外透过率曲线图;
图3是本发明实施例1的硫系玻璃镜片红外透过率曲线图;
图4是本发明实施例2的硫系玻璃镜片红外透过率曲线图。
具体实施方式
一种镀金刚膜的红外硫系玻璃镜片,其红外硫系玻璃镜片的表面由内至外依次设置第一Ge膜层、第一ZnSe膜层、第二Ge膜层、第二ZnSe膜层、YF3膜层和AlSi膜层。镀金刚膜的红外硫系玻璃镜片的结构示意图可参见附图1。
优选的,第一Ge膜层的厚度为215~225nm,第一ZnSe膜层的厚度为460~470nm,第二Ge膜层的厚度为230~240nm、第二ZnSe膜层的厚度为420~430nm、YF3膜层的厚度为1220~1240nm,AlSi膜层的厚度为230~240nm。
一种镀金刚膜的红外硫系玻璃镜片的制备方法,是将待镀膜的红外硫系玻璃镜片清洗,烘烤后,依次在镜片表面蒸镀第一Ge膜、第一ZnSe膜、第二Ge膜、第二ZnSe膜、YF3膜和AlSi膜,然后再烘烤制成。
制备方法中,优选的,蒸镀AlSi膜所用的膜料为Al2O3和SiO2组成的AlSi混合物。
进一步优选的,AlSi混合物在550nm下的折射率为1.46~1.50;再进一步优选的,AlSi混合物在550nm下的折射率为1.48;所述的AlSi混合物优选自阿石创MU1铝硅混合物材料。
制备方法中,优选的,清洗为离子清洗机清洗。
制备方法中,优选的,离子清洗机的离子源为氩气。
制备方法中,优选的,清洗的时间为15~50min。
制备方法中,优选的,蒸镀前,烘烤的温度为80~180℃,烘烤的时间为50~120min。
制备方法中,优选的,蒸镀后,烘烤的温度为80~120℃,烘烤的时间为50~150min。
以下通过具体的实施例对本发明的内容作进一步详细的说明。
实施例1~4中蒸镀AlSi膜层所用的膜料均为阿石创MU1铝硅混合物材料,其在550nm下的折射率为1.48,透明波段为300~7000nm。所用蒸镀Ge层、ZnSe层和YF3层的膜料为本领域的常见光学膜料,可由市面购买得到。
实施例1:
将待镀膜的红外硫系玻璃镜片置于蒸镀镀膜机中,待体系压力小于3×10-4Pa后,用氩离子源请扫30min后,在150℃下烘烤60min,然后依次在镜片表面蒸镀222nm厚的第一Ge膜层、466nm厚的第一ZnSe膜层、235nm厚的第二Ge膜层、423nm厚的第二ZnSe膜层、1230nm厚的YF3膜层和232nm厚的AlSi膜层,蒸镀完后再在100℃下烘烤70min,制成实施例1的镀金刚膜的红外硫系玻璃镜片。
实施例2:
将待镀膜的红外硫系玻璃镜片置于蒸镀镀膜机中,待体系压力小于3×10-4Pa后,用氩离子源请扫40min后,在80℃下烘烤120min,然后依次在镜片表面蒸镀216nm厚的第一Ge膜层、461nm厚的第一ZnSe膜层、232nm厚的第二Ge膜层、427nm厚的第二ZnSe膜层、1222nm厚的YF3膜层和236nm厚的AlSi膜层,蒸镀完后再在120℃下烘烤50min,制成实施例2的镀金刚膜的红外硫系玻璃镜片。
实施例3:
将待镀膜的红外硫系玻璃镜片置于蒸镀镀膜机中,待体系压力小于3×10-4Pa后,用氩离子源请扫15min后,在110℃下烘烤80min,然后依次在镜片表面蒸镀220nm厚的第一Ge膜层、468nm厚的第一ZnSe膜层、231nm厚的第二Ge膜层、421nm厚的第二ZnSe膜层、1238nm厚的YF3膜层和239nm厚的AlSi膜层,蒸镀完后再在80℃下烘烤150min,制成实施例3的镀金刚膜的红外硫系玻璃镜片。
实施例4:
将待镀膜的红外硫系玻璃镜片置于蒸镀镀膜机中,待体系压力小于3×10-4Pa后,用氩离子源请扫50min后,在180℃下烘烤50min,然后依次在镜片表面蒸镀218nm厚的第一Ge膜层、463nm厚的第一ZnSe膜层、239nm厚的第二Ge膜层、429nm厚的第二ZnSe膜层、1234nm厚的YF3膜层和235nm厚的AlSi膜层,蒸镀完后再在100℃下烘烤80min,制成实施例4的镀金刚膜的红外硫系玻璃镜片。
对比例1:
在待镀膜的红外硫系玻璃镜片只蒸镀一层150nm厚的氧化铝膜作为对比例,其余条件与实施例1的相同。
附图2、3和4分别为本发明对比例1、实施例1和实施例2的硫系玻璃镜片红外透过率曲线图。通过图2~3结果可知,对比例1的镀氧化铝膜的硫系玻璃镜片在红外波长8~12μm的范围内,其透过率Tave低于80%,而实施例1的镀金刚膜的硫系玻璃镜片在红外波长8~12μm的范围内,其透过率均≥95%。从图4可知,实施例2在红外波长8~12μm的范围内,其透过率Tave也≥95%。在红外波长8~12μm的范围内,实施例1的透过率平均值为97.16%,实施例2的透过率平均值为96.76%。
根据GB/T 32559-2016对实施例1~4的镀金刚膜的红外硫系玻璃镜片分别进行附着力测试、高温高湿测试、低温测试和高低温冲击试验。
1、附着力测试
测试工具:LP-24胶带
测试方法:用LP-24胶带粘附在陪镀片膜层表面,胶带粘附位置为陪镀片的对角线或直径,然后垂直于膜层表面方法的力迅速拉起一次。
测试结果:11W台灯下反射目视检查陪镀片膜层表面质量,实施例1~4在测试后均无变化无膜脱,附着力测试合格。
2、高温高湿测试
测试设备:恒温恒湿试验机
测试条件:高温高湿实验(60℃90%RH,72h)
测试结果:11W台灯下反射目视检查陪镀片膜层表面质量,后再测试附着力。结果表明,实施例1~4在高温高湿测试后,膜层表面均无变化;附着力测试前后无变化无膜脱,附着力合格。所以,实施例1~4的高温高湿测试合格。
3、低温测试
测试设备:恒温恒湿试验机
测试条件:低温实验(-40℃,72h)
测试结果:11W台灯下反射目视检查陪镀片膜层表面质量,后再测试附着力。结果表明,实施例1~4在低温测试后,膜层表面均无变化;附着力测试前后无变化无膜脱,附着力合格。所以,实施例1~4的低温测试合格。
4、高低温冲击试验
测试设备:冷热冲击试验机
测试条件:高低温冲击实验(70℃~-40℃各20min,3个循环)
测试结果:11W台灯下反射目视检查陪镀片膜层表面质量,后再测试附着力。结果表明,实施例1~4在高低温冲击试验后,膜层表面均无变化;附着力测试前后无变化无膜脱,附着力合格。所以,实施例1~4的高低温冲击试验合格。
综上,本发明在红外硫系玻璃表面镀制依红外光学薄膜光谱透过率规格需求设计特殊膜系,使用特殊膜料不同膜厚度搭配及设定特殊条件下专用镀膜机台蒸镀,并使镀制的薄膜最面层镀制AlSi金刚膜;所镀制的红外光学薄膜在实现满足红外光学薄膜光谱透过规格要求8~12μm透过率Tave≥95%,同时一次性实现红外硫系玻璃镜片耐磨擦性光学薄膜,经验证所蒸镀制的红外光学薄膜已完全达到金刚膜需求效果。
Claims (9)
1.一种镀金刚膜的红外硫系玻璃镜片,其特征在于:红外硫系玻璃镜片的表面由内至外依次设置第一Ge膜层、第一ZnSe膜层、第二Ge膜层、第二ZnSe膜层、YF3膜层和AlSi膜层;所述第一Ge膜层的厚度为215~225nm,第一ZnSe膜层的厚度为460~470nm,第二Ge膜层的厚度为230~240nm、第二ZnSe膜层的厚度为420~430nm、YF3膜层的厚度为1220~1240nm,AlSi膜层的厚度为230~240nm。
2.权利要求1所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:将待镀膜的红外硫系玻璃镜片清洗,烘烤后,依次在镜片表面蒸镀第一Ge膜、第一ZnSe膜、第二Ge膜、第二ZnSe膜、YF3膜和AlSi膜,然后再烘烤制成。
3.根据权利要求2所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:蒸镀AlSi膜所用的膜料为Al2O3和SiO2组成的AlSi混合物。
4.根据权利要求3所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:AlSi混合物在550nm下的折射率为1.46~1.50。
5.根据权利要求2所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:清洗为离子清洗机清洗。
6.根据权利要求5所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:离子清洗机的离子源为氩气。
7.根据权利要求6所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:清洗的时间为15~50min。
8.根据权利要求2所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:蒸镀前,烘烤的温度为80~180℃,烘烤的时间为50~120min。
9.根据权利要求2所述的一种镀金刚膜的红外硫系玻璃镜片的制备方法,其特征在于:蒸镀后,烘烤的温度为80~120℃,烘烤的时间为50~150min。
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