CN110007377B - 一种皮秒激光高功率增透膜及其制备方法 - Google Patents
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Abstract
本发明公开了一种皮秒激光高功率增透膜及其制备方法，一种皮秒激光高功率增透膜，包括基底层，基底层上交替沉积有HfO2层和SiO2层，HfO2层和SiO2层的层数相等。本发明皮秒激光高功率增透膜，通过膜材料及结构的改进，在1064波段透过率可达99.8%以上，650波段透过率可达98%以上，具有较高的激光损伤阈值，同时又具有高耐磨强度和高附着力，稳定性好，可满足目前激光领域的一些高端应用；制备重复性好，过程简单易操作、易控制。
Description
技术领域
本发明涉及一种皮秒激光高功率增透膜及其制备方法，属于皮秒激光增透膜领域。
背景技术
皮秒激光是一款脉宽为皮秒的激光器，具有皮秒级超短脉宽、重复频率可调、脉冲能量高等特点，在生物医学、光学参量振荡、生物显微成像等领域有着越来越广泛的应用，逐渐成为现代生物成像和分析系统中日益重要的工具。
在光学元件中，由于元件表面的反射作用而使光能损失，为了减少元件表面的反射损失，常在光学元件表面镀层透明介质薄膜，这种薄膜就叫增透膜。
现有的增透膜在皮秒激光应用上，多存在易烧膜，不耐用，抗激光损伤阈值低的情况。
发明内容
本发明提供一种皮秒激光高功率增透膜及其制备方法，通过对膜料的合理选择及结构的合理设计，使得到的膜层既有良好的光谱性能又有较好的机械稳性能和稳定性。
为解决上述技术问题，本发明所采用的技术方案如下：
一种皮秒激光高功率增透膜，包括基底层，基底层上交替沉积有HfO2层和SiO2层，HfO2层和SiO2层的层数相等。
上述Hf为铪。
申请人经研究发现，薄膜吸收激光能量产生热效应，使自身温度升高，且短时间内急剧加热，在局部热点周围产生热弹性压力和应力波加剧了薄膜的最终破坏；所以必须选择吸收小的材料，减少热效应的影响；低折射率材料选用SiO2(折射率=1.46)，膜层结构为无定形态，在工作波长上色散较小，小光系数低，吸收少，具有较高的激光损伤阈值；高折射率材料有TiO2、ZrO2和HfO2，TiO2在电子枪加热蒸发过程中极易分解，生成低阶氧化物，使膜层的吸收明显增大，ZrO 材料在沉积过程中蒸发速率不稳定，容易形成大的颗粒，且折射率不稳定，散射损耗随之增大；HfO2阈值较高，吸收较少，但蒸镀时易喷溅，本申选用不易喷溅的金属铪在氧气环境反应蒸发的方法，即具有HfO2的良好性能，又可以避免易喷溅的缺点。
基底层优选为石英玻璃基底层。
本申请给出了一种在石英基板表面蒸镀可见光和近红外双波段具有高抗激光损伤阈的激光高功率增透膜，该增透膜在1064波段透过率可达99.8%以上，650波段透过率可达98%以上，具有较高的激光损伤阈值，可满足目前激光领域的一些高端应用；且机械性能好，稳定性强。
为了兼顾增透膜的光谱性能、机械性能和成本，优选，HfO2层和SiO2层的层数均为2-5层。
进一步优选，f层和SiO2层的层数均为2层，也即皮秒激光高功率增透膜包括基底层，基底层上依次沉积有第一HfO2层、第一SiO2层、第二HfO2层和第二SiO2层。
为了兼顾增透膜的光谱性能和机械性能，优选，第一HfO2层的厚度小于第二HfO2层的厚度；第一SiO2层的厚度大于第二SiO2层的厚度；第一HfO2层的厚度小于第二SiO2层的厚度，第二HfO2层的厚度介于第二SiO2层的厚度和第一SiO2层的厚度之间。这样膜层相互间应力互补效果好，光谱性能和机械性能能得到更好的保障。
为了兼顾增透膜的光谱性能和机械性能，进一步优选，第一HfO2层的光学厚度为319.2±10nm，第一SiO2层的光学厚度为2447.2±10nm，第二HfO2层的光学厚度为1170.4±10nm，第二SiO2层的光学厚度为1032.08±10nm。
也即优选的膜层结构设计为：SUB/ k1Hk2Lk3Hk4L /A，其中SUB代表JGS1基底、A代表空气、H代表Hf、L代表SiO2；k1-k4代表每层的四分之一参考波长（1064nm）光学厚度的系数,分别为0.3/2.3/1.1/0.97。
本申请皮秒激光高功率增透膜的制备，采用离子源辅助电子束蒸发方法在基底层依次交替沉积HfO2层和SiO2层。
为了确保增透膜的光谱性能和机械性能，本申请皮秒激光高功率增透膜的制备方法，包括如下步骤：
1）对铪和SiO2膜料进行单独预熔处理，去除膜料内部的杂质；
2）将基底层清洁后，置于真空室内，在真空室内压强为（1.8±0.2）× 10-3Pa 、烘烤温度为250-300℃的条件下，采用离子源辅助电子束蒸发方法在基底层的表面依次沉积复合层和MgF2层。
为了提高膜的附着力，步骤2）中，基底层清洁方法为：将基底层表面进行超光滑表面抛光，使表面粗糙度Ra小于5埃，镀膜前对基片表面进行超声波清洗，去除基板表面附着的微观颗粒，使膜层附着性更强。
为了提升膜质量，步骤2）中，沉积时，在真空室导入氧化能力比普通分子态氧气更强的高纯氧气（≥99.99%）使得沉积材料在高真空状态下能得到充分氧化，并在射频源的作用下，提高成膜致密性，降低了薄膜的吸收，从而提高抗激光损伤阈值。此方法不但保留了电子束热蒸发方法制备激光薄膜独有的有利的性能又同时改善了薄膜的本征吸收和缺陷密度，具有针对性强、品质高、简单易行的特点。
进一步优选，沉积HfO2层时，所用原料为高纯氧气和Hf，高纯氧气的充气量为150-180sccm；沉积SiO2时，高纯氧气的充气量为60-100sccm。
优选，离子源束流为20A。
为了确保膜质量，优选，Hf的蒸发速率为0.15±0.02nm/S，SiO2的蒸发速率为1±0.02nm/S。
本发明未提及的技术均参照现有技术。
本发明皮秒激光高功率增透膜，通过膜材料及结构的改进，在1064波段透过率可达99.8%以上，650波段透过率可达98%以上，具有较高的激光损伤阈值，同时又具有高耐磨强度和高附着力，稳定性好，可满足目前激光领域的一些高端应用；制备重复性好，过程简单易操作、易控制。
附图说明
图1 为实施例1中皮秒激光高功率增透膜的结构示意图（图中省略了基底层）；
图2为实施例1中皮秒激光高功率增透膜的双面透过率设计曲线；
图3为实施例1中皮秒激光高功率增透膜的单面反射率设计曲线；
图4为实施例1中皮秒激光高功率增透膜的实测光谱曲线图（a为双面透过率，b为单面反射率）；
图中，1为基底层侧，2为第一HfO2层，3为第一SiO2层，4为第二HfO2层，5为第二SiO2层，6为空气侧。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本发明的内容不仅仅局限于下面的实施例。
镀膜设备选用日本昭和镀膜机（SGC-S1300Ci），配有双冷凝泵（ULVAC RBH-22），Polycold(PFC-1102 HC)，双电子枪（日新技研 NEB-10WE型）以及射频离子源（SER.NO 12-4088）；
实施例1
如图1所示，一种皮秒激光高功率增透膜，包括基底层，基底层上依次沉积有第一HfO2层、第一SiO2层、第二HfO2层和第二SiO2层，基底层为厚度为2mm的石英玻璃基底层。
第一HfO2层的光学厚度为319.2nm，第一SiO2层的光学厚度为2447.2nm，第二HfO2层的光学厚度为1170.4nm，第二SiO2层的光学厚度为1032.08nm。
上述皮秒激光高功率增透膜的制备方法，包括如下步骤：
1）对铪和SiO2膜料进行单独预熔处理，去除膜料内部的杂质；
2）将基底层表面进行超光滑表面抛光，使表面粗糙度Ra小于5埃，然后超声波清洗，再置于真空室内，在真空室内压强为1.8×10-3Pa 、烘烤温度为280℃的条件下，采用离子源辅助电子束蒸发方法在基底层的表面依次沉积复合层和MgF2层，沉积时，在真空室导入高纯氧气使得沉积材料在高真空状态下能得到充分氧化，并在射频源的作用下，提高成膜致密性，降低了薄膜的吸收，从而提高抗激光损伤阈值，沉积HfO2层时所用原料为高纯氧气和Hf，高纯氧气的充气量为150-180sccm；沉积SiO2时，高纯氧气的充气量为60-100sccm，离子源束流为20A；Hf的蒸发速率为0.15nm/S, SiO2的蒸发速率为1nm/S。通过在蒸发源与基底层之间加隔离挡板，阻挡并吸附无效的蒸发材料，减少了基底层附近的污染，降低了薄膜缺陷形成的几率。
采用白俄罗斯的PHOTO RT分光光度计对本例增透膜的单面反射率和双面透过率进行了测试，得到的光谱曲线达到设计要求，见图4，图2-3为设计曲线。
现有的PVD镀膜，激光损伤阈值最高可以达到28.4J/cm2(激光脉冲宽度10ns，1-on-1检测方式)，而本例增透膜的实测结果为40J/cm2（委托美国Spica Technologies Inc.公司检测）；本例的增透膜，用波长1064nm脉冲宽度6ps的激光在重复频率10KHZ时的激光损伤阈值达到12J/cm2。
实施例2
一种皮秒激光高功率增透膜，包括基底层，基底层上依次沉积有第一HfO2层、第一SiO2层、第二HfO2层和第二SiO2层，基底层为厚度为2mm的石英玻璃基底层。第一HfO2层的光学厚度为320.5nm，第一SiO2层的光学厚度为2450.3nm，第二HfO2层的光学厚度为1172.6nm，第二SiO2层的光学厚度为1030.8nm。
上述皮秒激光高功率增透膜的制备方法参照实施例1。本例的增透膜，用波长1064nm脉冲宽度6ps的激光在重复频率10KHZ时的激光损伤阈值达到12J/cm2。
将上述各例所得膜按照GJB2485-95光学膜层通用规范的要求，进行如下环境试验：
(1)耐磨强度实验：在橡皮摩擦头外裹2层干燥脱脂纱布，保持4.9 N压力下顺着同一轨迹对膜层进行摩擦，往返25次，膜层均无擦痕等损伤。
(2)附着力实验：用宽为2 cm，剥离强度I>2.94 N／cm 的胶带纸粘牢在膜层表面，将胶带纸从零件的边缘朝表面的垂直方向迅速拉起后，膜层均无脱落、无损伤。
(3)浸泡试验：将样品完全浸入蒸馏水或去离子水中，96小时后膜层均不出现新的起皮、剥离、裂纹、起泡等缺陷。
结论：上述各例采用超声波辅助清洗技术，通过膜料的合理选择与设计，使得到的膜层既有良好的光谱性能又有较好的机械稳性能和稳定性。
Claims (6)
1.一种皮秒激光高功率增透膜的制备方法，其特征在于：皮秒激光高功率增透膜包括基底层，基底层上依次沉积有第一HfO2层、第一SiO2层、第二HfO2层和第二SiO2层；
第一HfO2层的厚度小于第二HfO2层的厚度；第一SiO2层的厚度大于第二SiO2层的厚度；第一HfO2层的厚度小于第二SiO2层的厚度，第二HfO2层的厚度介于第二SiO2层的厚度和第一SiO2层的厚度之间；
基底层为石英玻璃基底层；
皮秒激光高功率增透膜制备时，采用离子源辅助电子束蒸发方法在基底层依次交替沉积HfO2层和SiO2层；
沉积HfO2层时，所用原料为高纯氧气和Hf，高纯氧气的充气量为150-180sccm，Hf的蒸发速率为0.15±0.02nm/S。
2.如权利要求1所述的制备方法，其特征在于：第一HfO2层的光学厚度为319.2±10nm，第一SiO2层的光学厚度为2447.2±10nm，第二HfO2层的光学厚度为1170.4±10nm，第二SiO2层的光学厚度为1032.08±10nm。
3.如权利要求1或2所述的制备方法，其特征在于：包括如下步骤：
1）对铪和SiO2膜料进行单独预熔处理，去除膜料内部的杂质；
2）将基底层清洁后，置于真空室内，在真空室内压强为（1.8±0.2）× 10-3Pa 、烘烤温度为250-300℃的条件下，采用离子源辅助电子束蒸发方法在基底层的表面依次沉积HfO2层和SiO2层。
4.如权利要求3所述的制备方法，其特征在于：步骤2）中，基底层清洁方法为：将基底层表面进行超光滑表面抛光，使表面粗糙度Ra小于5埃，然后超声波清洗；沉积时，在真空室导入高纯氧气使得沉积材料在高真空状态下能得到充分氧化。
5.如权利要求4所述的制备方法，其特征在于：步骤2）中，沉积SiO2时，高纯氧气的充气量为60-100sccm。
6.如权利要求3所述的制备方法，其特征在于：步骤2）中，离子源束流为20A； SiO2的蒸发速率为1±0.02nm/S 。
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