CN109097753A - 硫化锌窗口上高附着力硬质保护薄膜的制备方法 - Google Patents

硫化锌窗口上高附着力硬质保护薄膜的制备方法 Download PDF

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CN109097753A
CN109097753A CN201811003222.3A CN201811003222A CN109097753A CN 109097753 A CN109097753 A CN 109097753A CN 201811003222 A CN201811003222 A CN 201811003222A CN 109097753 A CN109097753 A CN 109097753A
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zinc sulphide
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薛俊
姚细林
张天行
杨放
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Hubei Jiuzhiyang Infrared System Co Ltd
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Abstract

本发明公开了一种硫化锌窗口上高附着力硬质保护薄膜的制备方法。在基片上由高纯度硫化锌膜料真空热蒸发而成，并采用离子束辅助沉积，其厚度为20～60nm；在连接层的基础上由高纯度氧化锌膜料电子枪蒸发而成，并采用离子束辅助沉积，厚度为40～70nm；随即放置于有氧环境的高温退火炉中进行退火处理；采用脉冲电源非平衡反应磁控溅射技术制备，沉积高硬度HfOxNy保护薄膜。本发明于保证光学性能的情况下进一步提高氮氧化铪薄膜的硬度，并解决氮氧化铪薄膜与硫化锌衬底的匹配问题，提高膜基牢固度。

Description

硫化锌窗口上高附着力硬质保护薄膜的制备方法
技术领域
本发明属于光学薄膜技术领域，具体涉及一种硫化锌窗口上高附着力硬质保护薄膜的制备方法。
背景技术
光学窗口是光学系统与外部恶劣环境相接触的光学零部件，在保证光学性能的同时，对零件的抗恶劣环境能力具备十分苛刻的要求。
硫化锌多晶材料具有优良的光学和力学性能，是一种先进的多光谱窗口、头罩和透镜材料。尽管在光学性能上具有独一无二的优势，但是这种窗口材料机械性能很差，硬度较低,仅为2.3GPa，在恶劣环境中使用时其光学表面易受到损伤而使红外透过率急剧下降,导致系统失效。因此,在实际使用过程中,硫化锌的窗口和头罩表面必须镀制保护膜,才能够保证其内部的光电探测系统能够正常工作。但硫化锌基底上沉积硬质薄膜(或膜系)往往附着力不足，以至于不能通过国军标要求的泡水、重度摩擦、盐雾、抗沙尘，抗雨蚀要求。因此需要寻找一种既有保护作用，又能够在可见光，中波红外和长波红外具有较高透过率，并且与硫化锌衬底有很好结合力的膜层或膜系。
氮氧化铪薄膜在可见光直到长波红外波段都有较好的透过率，适合作为多光谱涂层，目前文献报道北京有色金属研究院以N2和O2作为工作气体，采用磁控溅射制备的氮氧化铪硬度达到16GPa，但是这个硬度不能满足较高要求的抗沙尘要求。实验研究发现氧化物和氮氧化物薄膜直接在硫化锌衬底上沉积存在附着力差的问题。
发明内容
本发明目的在于保证光学性能的情况下进一步提高氮氧化铪薄膜的硬度，并解决氮氧化铪薄膜与硫化锌衬底的匹配问题，提高膜基牢固度。
为达到上述目的，采用技术方案如下：
硫化锌窗口上高附着力硬质保护薄膜的制备方法，包括以下步骤：
1)连接层的制备
在基片上由高纯度硫化锌膜料真空热蒸发而成，并采用离子束辅助沉积，其厚度为20～60nm；
2)匹配层的制备
在连接层的基础上由高纯度氧化锌膜料电子枪蒸发而成，并采用离子束辅助沉积，厚度为40～70nm；随即放置于有氧环境的高温退火炉中进行退火处理；
3)高硬度HfOxNy保护薄膜的制备
采用脉冲电源非平衡反应磁控溅射技术制备，以N2O作为反应前驱气体，Ar作为工作气体，工作气压0.1～1Pa，电源功率2000～3000W，脉冲频率80～160Hz，沉积温度350～450℃，靶压控制点为250～295V，N2O为根据靶压自动控制，反应溅射高纯Hf靶，沉积高硬度HfOxNy保护薄膜。
按上述方案，还包括在匹配层的制备前采用Ar和O2离子束对连接层进行离子轰击，活化表面并形成超薄氧化层。
按上述方案，步骤2退火处理温度设定为270～450℃，退火时间5～12小时。
按上述方案，所述HfOxNy保护薄膜是HfO2、HfON以及HfN的混合物膜层。
本发明中，首先在硫化锌窗口表面采用离子束辅助蒸发沉积方法制备ZnO/ZnS双层结构(即连接层和匹配层)，增加HfOxNy保护薄膜与衬底之间的结合力。双层结构包括同质连接层ZnS和匹配层ZnO，其中在ZnS同质连接层完成后进行Ar和O2混合离子束轰击，活化连接层表面并形成超薄氧化层，与匹配层处于更好的连接状态。
完成ZnO/ZnS双层结构连接匹配膜层后，对其进行退火工艺，提高ZnO膜层的氧化程度，改善光学性能。
采用非平衡反应磁控溅射技术制备高硬度HfOxNy保护薄膜，以纯度(99.99％)N2O作为反应前驱气体，纯度(99.99％)Ar作为工作气体，选择反应溅射过渡区30％处靶压，反应溅射高纯Hf靶(99.99％)，制备高硬度HfOxNy保护薄膜。以N2O作为氮氧源，可有效提高HfON成分的比例，在保证透过率的前提下提高膜层硬度。所得HfOxNy保护薄膜，具有很高的N含量(13.6％)，硬度高(20.46GPa)，致密性好，附着力好，能够对硫化锌窗口起到非常好的保护。
本发明的主要优点在于：
1)综合考虑硫化锌衬底的晶格尺寸和热膨胀系数，设计了一种具有双层结构的连接匹配层的膜系ZnS substrate/连接匹配层/HfOxNy，很好的解决了在硫化锌衬底表面制备HfOxNy薄膜因晶格失配和热失配引起的牢固度问题；同时对连接匹配层进行氧气氛围下退火，解决了蒸发制备连接匹配层中ZnO膜层时失氧的问题，改善了光学性能。
2)以N2O同时作为N源和O源的前驱气体，利用非平衡反应磁控溅射制备出高硬度HfOxNy多光谱薄膜。N2O作为反应气体，离化率高，相对于使用O2和N2作为反应气体，N2O有效分解N+和NO-离子比例高，因为N≡N键能相对比较高，需要的离化能较高。并且Hf–N成键需要的能量相比Hf–O和Hf–ON要高，因此使用O2和N2作为反应气体时，薄膜中HfO2成分比例高，N含量相对较低。N2O作为反应气体，溅射生成N原子百分比高达13.6％的HfOxNy薄膜，其硬度达到20.46GPa。相对于采用O2和N2作为气源，力学性能有了较大提高；
3)本发明中制备HfOxNy薄膜采用固定功率和气压，依靠自动控制氧气流量，维持固定反应溅射过渡区靶压，可以获得稳定成分的HfOxNy薄膜，即稳定的光学常数和沉积速率。并且具有非常好的重复性。
4)在硫化锌窗口上制备的ZnS substrate/连接匹配层/HfOxNy保护膜系，在可见光，近红外，中波红外以及长波红外都有较好的透过率，平均透过率高于硫化锌窗口本身透过率，不仅可以起到保护的作用，又有一定的增透作用。
5)在硫化锌窗口上制备的ZnS substrate/连接匹配层/HfOxNy保护膜系，对硫化锌窗口有很好的保护作用。可通过国军标GJB2485-1995光学膜层通用规范的要求其进行了低温-62℃、高温70℃、湿热50℃、95％RH以及盐雾试验。试验后，膜层无起皱、气泡、脱落、龟裂等现象；使用2cm宽胶带粘在其表面，垂直迅速拉起，膜层完好，无脱膜现象；使用压力9.8N的手持式摩擦器，橡胶擦头外裹脱脂布，在其表面摩擦40次，膜层完好，无擦痕等损伤痕迹。
附图说明
图1：实施例1中ZnO匹配层退火前后透过率曲线；
图2：实施例1中ZnS substrate/连接匹配层/HfOxNy膜系透过率曲线；
图3：实施例1中HfOxNy薄膜XPS测试曲线；
图4：实施例1中HfOxNy薄膜硬度测试曲线。
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。
实施例1
ZnS连接层镀制：将硫化锌衬底装入离子束辅助蒸发沉积镀膜机，开启离子源对硫化锌衬底表面进行离子束轰击，工作气体为高纯氩气(纯度99.99％)。离子源参数设置如下：偏压160V，放电电流50A，持续时间5分钟；然后沉积ZnS连接层，沉积速率0.20nm/s，物理厚度40nm。离子源参数设置：偏压125V，放电电流50A，进入离子源的氩气流量为15sccm；沉积完成后，开启离子源对ZnS连接层进行离子束轰击，离子源参数设置：偏压150V，放电电流30A，工作气体为高纯氩气(纯度99.99％)和高纯氧气(纯度99.99％)，氩气和氧气流量为20sccm/30sccm，混合离子束轰击5分钟。
ZnO匹配层镀制：ZnO匹配层沉积，沉积速率0.20nm/s，物理厚度60nm，离子源参数设置如下：偏压160V，放电电流50A，进入离子源的氩气和氧气流量为15sccm/20sccm。沉积完成后关闭离子源及工作气体继续抽真空，至基片温度降至80℃以下，打开蒸发室取件。
随即放置于有氧环境的高温退火炉中进行退火处理。温度设定为320℃，保温时间8小时。自然冷却至常温后取出。退火前后透过率光谱性能如图1所示，退火后可见光波段透过率有一定程度的改善，近红外直至长波红外波段透过率有非常大的提高。
高硬度HfOxNy保护薄膜的制备：将完成连接匹配层的硫化锌衬底装入脉冲电源非平衡反应磁控溅射镀膜机沉积HfOxNy薄膜之前，将温度设置为380℃，保温60分钟。然后设置Ar流量分别为40sccm，工作气压0.3Pa，电源功率2500W，脉冲频率130Hz靶压控制点为287V，N2O为根据靶压自动控制，预溅射10分钟，移开挡板，真空腔室中，N2O被离化N-、NO+以及O-离子，一部分在靶面反应并生成HfOxNy薄膜，然后被Ar离子溅射出来并沉积在基片上，一部分与溅射出来的Hf+在等离子区域反应生成HfOxNy薄膜并沉积在基片上。沉积时间120分钟。
本实施例所得ZnS substrate/连接匹配层/HfOxNy膜系透过率曲线性能测试采用Perkin Elmer 950分光光度计和Perkin Elmer Spectrum 100型傅里叶红外变换光谱仪(FTIR)进行测试，如图2所示，可见光、中波红外、长波红外波段平均透过率分别为：Tavg＝72.73％(0.45～0.78μm)；Tavg＝77.15％(3.7～4.8μm)；Tavg＝76.17％(7.7～10.3μm)。
采用ESCALAB 250Xi X射线光电子能谱仪(XPS)对HfOxNy保护薄膜进行了元素分析，如图3所示，N原子百分比为13.62％。
用MTS Nanolndenter XP纳米压痕仪测试了HfOxNy薄膜的硬度，如图4所示，显微硬度为20.6GPa。

Claims (4)

1.硫化锌窗口上高附着力硬质保护薄膜的制备方法，其特征在于包括以下步骤：
1)连接层的制备
在基片上由高纯度硫化锌膜料真空热蒸发而成，并采用离子束辅助沉积，其厚度为20～60nm；
2)匹配层的制备
在连接层的基础上由高纯度氧化锌膜料电子枪蒸发而成，并采用离子束辅助沉积，厚度为40～70nm；随即放置于有氧环境的高温退火炉中进行退火处理；
3)高硬度HfOxNy保护薄膜的制备
采用脉冲电源非平衡反应磁控溅射技术制备，以N2O作为反应前驱气体，Ar作为工作气体，工作气压0.1～1Pa，电源功率2000～3000W，脉冲频率80～160Hz，沉积温度350～450℃，靶压控制点为250～295V，N2O为根据靶压自动控制，反应溅射高纯Hf靶，沉积高硬度HfOxNy保护薄膜。
2.如权利要求1所述硫化锌窗口上高附着力硬质保护薄膜的制备方法，其特征在于还包括在匹配层的制备前采用Ar和O2离子束对所述连接层进行离子轰击，活化表面并形成超薄氧化层。
3.如权利要求1所述硫化锌窗口上高附着力硬质保护薄膜的制备方法，其特征在于步骤2退火处理温度设定为270～450℃，退火时间5～12小时。
4.如权利要求1所述硫化锌窗口上高附着力硬质保护薄膜的制备方法，其特征在于所述HfOxNy保护薄膜是HfO2、HfON以及HfN的混合物膜层。
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070264478A1 (en) * 2006-05-12 2007-11-15 Industrial Technology Research Institute Substrate structures for display application and fabrication methods thereof
CN102912293A (zh) * 2012-11-13 2013-02-06 中国航天科技集团公司第五研究院第五一0研究所 多光谱保护薄膜及其制备方法
CN103151459A (zh) * 2013-03-28 2013-06-12 天津理工大学 一种基于氮氧化铪低功耗阻变存储器及其制备方法
CN105223634A (zh) * 2015-09-18 2016-01-06 无锡泓瑞航天科技有限公司 一种2.5-10um谱段高透低应力薄膜及其制备方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070264478A1 (en) * 2006-05-12 2007-11-15 Industrial Technology Research Institute Substrate structures for display application and fabrication methods thereof
CN102912293A (zh) * 2012-11-13 2013-02-06 中国航天科技集团公司第五研究院第五一0研究所 多光谱保护薄膜及其制备方法
CN103151459A (zh) * 2013-03-28 2013-06-12 天津理工大学 一种基于氮氧化铪低功耗阻变存储器及其制备方法
CN105223634A (zh) * 2015-09-18 2016-01-06 无锡泓瑞航天科技有限公司 一种2.5-10um谱段高透低应力薄膜及其制备方法

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