CN116360017A - 一种硫系玻璃irg206基底长波红外镜片及其制备方法 - Google Patents
一种硫系玻璃irg206基底长波红外镜片及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种硫系玻璃IRG206基底长波红外镜片及其制备方法，适用的增透波段为8‑12um，属于红外光学领域。所述长波红外镜片以硫系玻璃IRG206为基底，基底的正反面均镀制了同种红外增透膜系结构：IRG206/0.251ZnS/0.285Ge/0.247ZnS/0.760Ge/0.359ZnS/0.880YbF3/0.419ZnS/空气。本发明ZnS作为第一层膜，起到基底和膜层结构之间的过渡作用，以此提高膜层的附着力，减少脱膜情况的发生；第二至第第六层膜采用透光性能好的Ge、ZnS和YbF3，增大透光率；最后将ZnS作为保护膜镀制在最外层，以此减少外界环境对内部膜层的影响。在镀膜过程中采用离子源辅助，提高膜层和基底间的结合性能，改善薄膜的生长质量，降低膜层的残余应力。
Description
技术领域
本发明涉及一种硫系玻璃IRG206基底长波红外镜片及其制备方法，属于红外光学领域。
背景技术
硫系玻璃一般指的是以VI族元素S、Se、Te等元素为主，与As、Ge、Sb、Ga等元素形成的化合物玻璃。其优点有折射率温度系数低、通过的波段宽以及消色差和消热差性能好等，是一类优异的红外光学材料，在红外光学方面应用广泛。且相对于Ge等红外光学材料而言，其制备成本更低，不论是在红外光学的研发方面还是产品制造方面都有着不错的替代性。对于现有的以硫系玻璃IRG206(As40Se60)为基底且镀膜的长波红外镜片，8-12um的透光率不足50％、膜层质量低，无法满足工作需求。
发明内容
本发明旨在改进现有技术，提供一种硫系玻璃IRG206(As40Se60)基底长波红外镜片及其制备方法，使得长波红外镜片透光率高、膜层质量高。
为实现上述目的，本发明是通过如下技术方案实现的：一种硫系玻璃IRG206基底长波红外镜片，适用的增透波段为8-12um，长波红外镜片以硫系玻璃IRG206为基底，基底正反面均镀制了同种红外增透膜系结构，红外增透膜系结构为：IRG206/0.251ZnS/0.285Ge/0.247ZnS/0.760Ge/0.359ZnS/0.880YbF3/0.419ZnS/空气，膜料前面的数字表示膜层厚度，单位为um。
优选地，IRG206基底的厚度为2mm。
一种硫系玻璃IRG206基底长波红外镜片的制备方法，包括如下步骤：
步骤一：基底预处理：清洁基底表面，在强光灯的照射下看不到有杂质即可，再将清洁好的基底装至镀膜机中；
步骤二：镀膜准备：将ZnS、Ge和YbF3膜料放入不同坩埚中，将镀膜机内抽真空，基底预热，依次对ZnS、Ge和YbF3膜料进行手动预熔，将镀膜真空室加热并保持恒温；
步骤三：镀膜：对ZnS，Ge,YbF3膜料在镀膜机中进行镀前预熔，然后采用电子束加热蒸发的方式根据膜系结构在基底正反两面依次镀制各膜层，镀膜温度为120℃，镀膜过程中使用霍尔离子源辅助镀制,膜料蒸发过程中实时调整蒸发速率，使其稳定，镀制结束后，当真空室内的温度低于50℃时，取出镜片。
具体地，步骤二具体为：清洁镀膜机真空室，清理蒸发源中的杂质，将ZnS、Ge和YbF3膜料放入不同的坩埚埚位中，将镀膜机内抽真空，打开烘烤，打开工转，烘烤工转为8转/分钟，其中，恒温温度为120℃，恒温时间为30-40min。烘烤基底，当烘烤温度达到120℃后，真空室内以该温度恒温30-40min，然后按照ZnS、Ge、YbF3的顺序，将坩埚内的膜料手动预熔到熔融状态：待室内真空度到达6*E-3Pa时候，坩埚位置调整到对应的膜料锅位，打开高压，关闭电子枪挡板，打开电子枪，调节电子枪束流大小、光斑大小以及光斑位置，对膜料进行预熔，直至膜料为熔融状态，关闭高压，关闭电子枪。
具体地，步骤三中：将ZnS，Ge,YbF3膜料在镀膜机中进行镀前预熔时，ZnS膜料预熔时的电子束电流和时间分别为20mA-40s，30mA-40s，Ge膜料预熔时的电子束电流和时间分别为120mA-30s、140mA-30s，YbF3膜料预熔时的电子束电流和时间分别为30mA-30s、40mA-30s；
具体地，步骤三中，在镀膜过程中使用霍尔离子源辅助镀制，离子源阳极电压为80v，阳极电流为0.6A，发射级电压为1.2A。
具体地，步骤三中，ZnS膜层采用电子束加热的方法镀制，电子束流为40mA，沉积速率为1.2nm/s，镀制时电子束的光斑直径为6-8mm。
具体地，步骤三中，Ge膜层采用电子束加热的方法镀制，电子束流为160mA，沉积速率为0.6nm/s，镀制时电子束的光斑直径为2-3mm。
具体地，步骤三中，YbF3膜层采用电子束加热的方法镀制，电子束流为50mA，沉积速率为0.8nm/s，镀制时电子束的光斑直径为14-16mm。
本发明的有益效果是：本发明红外镜片以硫系玻璃IRG206为基底，基底的正反面均镀制了同种红外增透膜系结构，膜系结构为7层不同材料的光学薄膜组成。在基底上由不同材料按照高折射率和低折射率相互匹配的方法依次沉积的多层膜系可以使光学镜片的透光率更大，镀制完成后的镜片透光率达到97％以上。本发明将较为致密、机械性能好且与硫系玻璃IRG206具有一定连接性的ZnS作为第一层膜，起到基底和膜层结构之间的过渡作用，以此提高膜层的附着力，减少脱膜情况的发生；第二至第六层膜采用透光性能好的Ge、ZnS、Ge、ZnS和YbF3，增大透光率；最后将ZnS作为保护膜镀制在最外层，以此减少外界环境对内部膜层的影响。在镀膜过程中采用离子源辅助，提高膜层和基底间的结合性能，改善薄膜的生长质量，降低膜层的残余应力。
附图说明
图1是本发明的膜系结构图；
图2是本发明中硫系玻璃IRG206的透光率曲线图
图3是本发明中成品的透光率曲线图。
具体实施方式
下面结合实施例和附图对本发明作进一步的说明，但不以任何方式对本发明加以限制，基于本发明教导所作的任何变换或替换，均属于本发明的保护范围。
实施例1：如图1-3所示，一种硫系玻璃IRG206基底长波红外镜片，适用的增透波段为8-12um，长波红外镜片以硫系玻璃IRG206为基底，基底正反面均镀制了同种红外增透膜系结构，红外增透膜系结构为：
IRG206/0.251ZnS/0.285Ge/0.247ZnS/0.760Ge/0.359ZnS/0.880YbF3/0.419ZnS/空气，膜料前面的数字表示膜层厚度，单位为um。
进一步地，IRG206基底的厚度为2mm。
一种硫系玻璃IRG206基底长波红外镜片的制备方法，包括如下步骤：
步骤一：基底预处理：使用傅里叶光谱仪检测IRG206基底的透光率，如图2所示，8-12um波段内的平均透过率为49％左右，清洁基底表面，在强光灯的照射下看不到有杂质即可，再将清洁好的基底装至镀膜机中；
步骤二：镀膜准备：将ZnS、Ge和YbF3膜料放入不同坩埚中，将镀膜机内抽真空，基底预热，依次对ZnS、Ge和YbF3膜料进行手动预熔，将镀膜真空室加热并保持恒温；
步骤三：镀膜：对ZnS，Ge,YbF3膜料在镀膜机中进行镀前预熔，然后采用电子束加热蒸发的方式根据膜系结构在基底正反两面依次镀制各膜层，镀膜温度为120℃，镀膜过程中使用霍尔离子源辅助镀制,膜料蒸发过程中实时调整蒸发速率，使其稳定，镀制结束后，当真空室内的温度低于50℃时，取出镜片。进一步地，步骤二具体为：清洁镀膜机真空室，清理蒸发源中的杂质，将ZnS、Ge和YbF3膜料放入不同的坩埚埚位中，将镀膜机内抽真空，打开烘烤，打开工转，烘烤工转为8转/分钟，其中，恒温温度为120℃，恒温时间为30-40min。烘烤基底，当烘烤温度达到120℃后，真空室内以该温度恒温30-40min，然后按照ZnS、Ge、YbF3的顺序，将坩埚内的膜料手动预熔到熔融状态：
预熔ZnS膜料：待室内真空度到达6*E-3Pa时候，坩埚位置调整到ZnS膜料锅位，打开高压，关闭电子枪挡板，打开电子枪，调节电子枪束流大小、光斑大小以及光斑位置，对ZnS膜料进行预熔，直至ZnS膜料为熔融状态，关闭高压，关闭电子枪。
预熔Ge膜料：ZnS膜料预熔完成后，坩埚位置调整到Ge膜料锅位，打开高压，关闭电子枪挡板，打开电子枪，调节电子枪束流大小、光斑大小以及光斑位置，对Ge膜料进行预熔，直至Ge膜料为熔融状态，关闭高压，关闭电子枪。
预熔YbF3膜料：Ge膜料预熔完成后，坩埚位置调整到YbF3膜料锅位，打开高压，关闭电子枪挡板，打开电子枪，调节电子枪束流大小、光斑大小以及光斑位置，对YbF3膜料进行预熔，直至YbF3膜料为熔融状态，关闭高压，关闭电子枪。
进一步地，步骤三中：将ZnS，Ge,YbF3膜料在镀膜机中进行镀前预熔时，ZnS膜料预熔时的电子束电流和时间分别为20mA-40s，30mA-40s，Ge膜料预熔时的电子束电流和时间分别为120mA-30s、140mA-30s，YbF3膜料预熔时的电子束电流和时间分别为30mA-30s、40mA-30s；
进一步地，步骤三中，在镀膜过程中使用霍尔离子源辅助镀制，离子源阳极电压为80v，阳极电流为0.6A，发射级电压为1.2A。
进一步地，步骤三中，ZnS膜层采用电子束加热的方法镀制，电子束流为40mA，沉积速率为1.2nm/s，镀制时电子束的光斑直径为6-8mm。
进一步地，步骤三中，Ge膜层采用电子束加热的方法镀制，电子束流为160mA，沉积速率为0.6nm/s，镀制时电子束的光斑直径为2-3mm。
进一步地，步骤三中，YbF3膜层采用电子束加热的方法镀制，电子束流为50mA，沉积速率为0.8nm/s，镀制时电子束的光斑直径为14-16mm。
对镀膜镜片进行性能测试如下：
透过率测试：使用傅里叶光谱仪测量镀膜镜片的透过率，如图3所示，8-12um波段内平均透过率大于97％。
附着力试验：按照GJB2485-1995标准3.4.1.1中的检测方法，使用3M胶带牢牢贴在膜层表面，垂直迅速拉起后，无脱膜现象。
湿热试验：将镀膜镜片放置在温度50℃，湿度95％湿热试验箱中，恒温恒湿静置24h后取出，取出后观察膜层表面，无变色、龟裂、脱膜现象。
高低温试验：将镀膜镜片放入高低温试验箱中，分别在-62℃的低温中和70℃的高温中静置2h，待其降至室温后取出，检测膜层均无起皮、起泡、裂纹、脱膜等现象。
耐磨试验：在橡皮摩擦头外包裹两层干燥脱脂纱布，保持4.9N压力下顺着同一轨迹对膜层进行摩擦，距离为20mm，往返25次，膜层均无擦痕等损伤。
最后说明的是，以上优选实施例仅用以说明本发明的技术方案而非限制，尽管通过上述优选实施例已经对本发明进行了详细的描述，但本领域技术人员应当理解，可以在形式上和细节上对其做出各种各样的改变，而不偏离本发明权利要求书所限定的范围。
Claims (9)
1.一种硫系玻璃IRG206基底长波红外镜片，其特征在于：适用的增透波段为8-12um，长波红外镜片以硫系玻璃IRG206为基底，基底正反面均镀制了同种红外增透膜系结构，红外增透膜系结构为：
IRG206/0.251ZnS/0.285Ge/0.247ZnS/0.760Ge/0.359ZnS/0.880YbF3/0.419ZnS/空气，膜料前面的数字表示膜层厚度，单位为um。
2.根据权利有要求1所述的一种硫系玻璃IRG206基底长波红外镜片，其特征在于：IRG206基底的厚度为2mm。
3.一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：包括如下步骤：
步骤一：基底预处理：清洁基底表面，在强光灯的照射下看不到有杂质即可，再将清洁好的基底装至镀膜机中；
步骤二：镀膜准备：将ZnS、Ge和YbF3膜料放入不同坩埚中，将镀膜机内抽真空，基底预热，依次对ZnS、Ge和YbF3膜料进行手动预熔，将镀膜真空室加热并保持恒温；
步骤三：镀膜：对ZnS，Ge,YbF3膜料在镀膜机中进行镀前预熔，然后采用电子束加热蒸发的方式根据膜系结构在基底正反两面依次镀制各膜层，镀膜温度为120℃，镀膜过程中使用霍尔离子源辅助镀制,膜料蒸发过程中实时调整蒸发速率，使其稳定，镀制结束后，当真空室内的温度低于50℃时，取出镜片。
4.根据权利要求3所述的一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：步骤二具体为：清洁镀膜机真空室，清理蒸发源中的杂质，将ZnS、Ge和YbF3膜料放入不同的坩埚埚位中，将镀膜机内抽真空，打开烘烤，打开工转，烘烤工转为8转/分钟，其中，恒温温度为120℃，恒温时间为30-40min。烘烤基底，当烘烤温度达到120℃后，真空室内以该温度恒温30-40min，然后按照ZnS、Ge、YbF3的顺序，将坩埚内的膜料手动预熔到熔融状态：待室内真空度到达6*E-3Pa时候，坩埚位置调整到对应的膜料锅位，打开高压，关闭电子枪挡板，打开电子枪，调节电子枪束流大小、光斑大小以及光斑位置，对膜料进行预熔，直至膜料为熔融状态，关闭高压，关闭电子枪。
5.根据权利要求3所述的一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：步骤三中：将ZnS，Ge,YbF3膜料在镀膜机中进行镀前预熔时，ZnS膜料预熔时的电子束电流和时间分别为20mA-40s，30mA-40s，Ge膜料预熔时的电子束电流和时间分别为120mA-30s、140mA-30s，YbF3膜料预熔时的电子束电流和时间分别为30mA-30s、40mA-30s。
6.根据权利要求3所述的一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：步骤三中，霍尔离子源阳极电压为80v，阳极电流为0.6A，发射级电压为1.2A。
7.根据权利要求3所述的一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：步骤三中，ZnS膜层采用电子束加热的方法镀制，电子束流为40mA，沉积速率为1.2nm/s，镀制时电子束的光斑直径为6-8mm。
8.根据权利要求3所述的一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：步骤三中，Ge膜层采用电子束加热的方法镀制，电子束流为160mA，沉积速率为0.6nm/s，镀制时电子束的光斑直径为2-3mm。
9.根据权利要求3所述的一种硫系玻璃IRG206基底长波红外镜片的制备方法，其特征在于：步骤三中，YbF3膜层采用电子束加热的方法镀制，电子束流为50mA，沉积速率为0.8nm/s，镀制时电子束的光斑直径为14-16mm。
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