CN110983279B - 一种高硬度低吸收氮化硅薄膜的制备方法 - Google Patents

一种高硬度低吸收氮化硅薄膜的制备方法 Download PDF

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CN110983279B
CN110983279B CN201911146631.3A CN201911146631A CN110983279B CN 110983279 B CN110983279 B CN 110983279B CN 201911146631 A CN201911146631 A CN 201911146631A CN 110983279 B CN110983279 B CN 110983279B
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刘华松
姜玉刚
何家欢
王利栓
季一勤
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Tianjin Jinhang Institute of Technical Physics
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Abstract

本发明涉及一种高硬度低吸收Si3N4薄膜的制备方法，属于光学薄膜技术领域。本发明提供一种高硬度低吸收离子束溅射Si3N4薄膜的制备方法，通过采用双离子束溅射沉积技术，通过改变主离子源和辅助离子源的工艺参数，以及真空室和辅助离子源通入氮气的流量，可实现高硬度低吸收Si3N4薄膜的制备。结果表明，该方法将大大提高Si3N4薄膜的硬度和降低吸收损耗，作为最外层保护薄膜，对于高性能中波红外硬质保护薄膜窗口的制备具有重要的作用。本发明对于不同离子源参数制备Si3N4薄膜具有普适性。

Description

一种高硬度低吸收氮化硅薄膜的制备方法
技术领域
本发明属于光学薄膜技术领域，具体涉及一种高硬度低吸收Si3N4薄膜的制备方法。
背景技术
随着红外技术的高速发展，红外制导武器的服役环境日益苛刻。红外窗口是红外热成像探测系统中的关键部件，位于红外成像系统的最前端。它是重要的结构/功能一体化部件，又是抗高速条件下的热力学冲击的薄弱环节。国外早在四十年代就开始了增透保护膜的研究和相关试验验证，但直到八十年代初国外才实现类金刚石保护膜(DLC膜)的沉积，试验表明保护膜对窗口表面的侵蚀耐受程度具有明显的提升。但DLC膜存在一定的吸收，在增透保护薄膜方面应用还存在一定的问题。
而由于作无定形态的Si3N4是一种重要的结构材料，它具有硬度高、弹性模量大，本身具有润滑性，表面摩擦系数小、耐磨损等特点，所以常被用作耐磨材料。同时它还具有耐高温、热膨胀系数小、导热系数大、抗热震性好，以及耐腐蚀、抗氧化等优点。所以Si3N4薄膜在硬质保护薄膜方面具有很大的应用前景。目前，制作氮化硅薄膜可以用化学气相沉积(CVD)、物理气相沉积(PVD)、离子束增强沉积 (IBED)、电子回旋共振等离子体化学气相沉积技术(ECR-PECVD) 以及射频和微波的等离子化学气相沉积(RF-PCVD和MW-PCVD) 等，但针对离子束溅射沉积技术制备Si3N4薄膜还鲜有报道。
综上所述，目前采用离子束溅射沉积技术制备Si3N4薄膜还未见报道。
发明内容
(一)要解决的技术问题
本发明要解决的技术问题是：如何实现高硬度低吸收Si3N4薄膜的制备。
(二)技术方案
为了解决上述技术问题，本发明提供了一种高硬度低吸收Si3N4薄膜的制备方法，包括以下步骤：
1)首先选择Si靶作为离子束溅射靶材；
2)其次采用离子束溅射沉积技术，在不同基底上制备Si3N4薄膜；
3)然后采用分光光度计和红外傅立叶光谱仪分别测量Si3N4薄膜的透射光谱；
4)基于透射光谱的反演方法，计算Si3N4薄膜的折射率和消光系数；
5)测量Si3N4薄膜的硬度。
优选地，步骤1中，选择熔融石英和Si基底作为Si3N4薄膜的沉积。
优选地，步骤2在制备时，选择镀膜真空室本体真空度为 m×10-6Torr，1≤m≤50，真空室氮气流量X为10≤X≤50，辅助离子源氮气流量Y为0～50sccm，主离子源工作参数为：工作电压U1为600V≤ U1≤1500V，工作电流I1为200mA≤I1≤900mA；辅助离子源工作参数为：工作电压U2为150V≤U2≤600V，工作电流I2为100mA≤I2≤400mA，在熔融石英和Si基底上制备Si3N4薄膜。
优选地，步骤2在制备时，选择镀膜真空室本体真空度为 4×10-6Torr，真空室氮气流量X为30sccm，辅助离子源氮气流量Y为 30sccm，主离子源工作参数：工作电压U1为1000V，工作电流I1为 450mA；辅助离子源工作参数：工作电压U2为300V，工作电流I2为200mA，在熔融石英和Si基底上制备Si3N4薄膜。
优选地，在熔融石英和Si基底上制备Si3N4薄膜时，膜层厚度为300nm。
优选地，步骤3中，采用分光光度计测量石英基底上Si3N4薄膜的可见光-近红外透过率曲线，测量范围为300nm-2500nm；采用红外傅立叶光谱仪测量Si基底上Si3N4薄膜的红外透过率曲线，测量范围为2500nm-20000nm。
优选地，步骤3中，采用Lambda900分光光度计测量石英基底上Si3N4薄膜的可见光-近红外透过率曲线。
优选地，步骤3中，采用PE红外傅立叶光谱仪测量Si基底上 Si3N4薄膜的红外透过率曲线。
优选地，步骤5中，采用纳米压痕法测量石英基底上Si3N4薄膜的硬度。
(三)有益效果
本发明提供一种高硬度低吸收离子束溅射Si3N4薄膜的制备方法，通过采用双离子束溅射沉积技术，通过改变主离子源和辅助离子源的工艺参数，以及真空室和辅助离子源通入氮气的流量，可实现高硬度低吸收Si3N4薄膜的制备。结果表明，该方法将大大提高Si3N4薄膜的硬度和降低吸收损耗，作为最外层保护薄膜，对于高性能中波红外硬质保护薄膜窗口的制备具有重要的作用。本发明对于不同离子源参数制备Si3N4薄膜具有普适性。
附图说明
图1为离子束溅射技术制备Si3N4薄膜工作示意图；
图2为石英基底上Si3N4薄膜的可见光-近红外透过率曲线图；
图3为Si基底上Si3N4薄膜的红外透过率曲线图；
图4为Si3N4薄膜的折射率曲线图；
图5为Si3N4薄膜的消光系数曲线图；
图6为Si3N4薄膜的硬度曲线图。
具体实施方式
为使本发明的目的、内容、和优点更加清楚，下面结合附图和实施例，对本发明的具体实施方式作进一步详细描述。
本发明提供了一种高硬度低吸收Si3N4薄膜的制备方法，包括以下步骤：
1)首先选择Si靶作为离子束溅射沉积靶材，选择熔融石英和Si 基底作为Si3N4薄膜的沉积基底；
2)采用双离子束溅射沉积技术，选择镀膜真空室本体真空度为 m×10-6Torr(1≤m≤50)，真空室氮气流量为Xsccm(10≤X≤50)，辅助离子源氮气流量为Y sccm(0≤Y≤50)，主离子源工作参数：工作电压为U1(600V≤U1≤1500V)，工作电流为I1(200mA≤ I1≤900mA)；辅助离子源工作参数：工作电压为U2 (150V≤U2≤600V)，工作电流为I2(100mA≤I2≤400mA)，在熔融石英和Si基底上制备Si3N4薄膜；
3)采用分光光度计测量石英基底上Si3N4薄膜的可见光-近红外透过率曲线，采用红外傅立叶光谱仪测量Si基底上Si3N4薄膜的红外透过率曲线；
4)采用基于透射光谱的光谱反演计算方法精确计算Si3N4薄膜的折射率和消光系数；
5)采用纳米压痕法测量石英基底上Si3N4薄膜的硬度。
下面以高硬度低吸收离子束溅射Si3N4薄膜制备为实例，具体步骤如下：
1)首先选择Si靶作为离子束溅射沉积靶材，选择熔融石英和Si 基底作为Si3N4薄膜的沉积；
2)采用双离子束溅射沉积技术，制备Si3N4薄膜工作示意图如图 1所示。选择镀膜真空室本体真空度为4×10-6Torr，真空室氮气流量X为30sccm，辅助离子源氮气流量Y为30sccm，主离子源工作参数：工作电压U1为1000V，工作电流I1为450mA；辅助离子源工作参数：工作电压U2为300V，工作电流I2为 200mA，在熔融石英和Si基底上制备了Si3N4薄膜，膜层厚度为300nm左右；
3)采用Lambda900分光光度计测量石英基底上Si3N4薄膜的可见光-近红外透过率曲线，测量范围为300nm-2500nm，测量结果如图2所示；采用PE红外傅立叶光谱仪测量Si基底上Si3N4薄膜的红外透过率曲线，测量范围为2500nm-20000nm，测量结果如图3所示；
4)采用基于透射光谱的光谱反演计算方法精确计算了Si3N4薄膜的折射率、消光系数、沉积速率等光学常数，折射率曲线如图 4所示，消光系数曲线如图5所示，在4000nm处的折射率和消光系数分别为1.916和2×10-4；
5)采用纳米压痕法测量石英基底上Si3N4薄膜的硬度，硬度曲线如图6所示，硬度值为19.79Gpa。
以上所述仅是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明技术原理的前提下，还可以做出若干改进和变形，这些改进和变形也应视为本发明的保护范围。

Claims (1)

1.一种高硬度低吸收Si3N4薄膜的制备方法，其特征在于，包括以下步骤：
1)首先选择Si靶作为离子束溅射靶材；
2)其次采用离子束溅射沉积技术，在不同基底上制备Si3N4薄膜；
3)然后采用分光光度计和红外傅立叶光谱仪分别测量Si3N4薄膜的透射光谱；
4)基于透射光谱的反演方法，计算Si3N4薄膜的折射率和消光系数；
5)测量Si3N4薄膜的硬度；
步骤1中，选择熔融石英和Si基底作为Si3N4薄膜的沉积；
步骤2在制备时，选择镀膜真空室本体真空度为4×10-6Torr，真空室氮气流量X为30sccm，辅助离子源氮气流量Y为30sccm，主离子源工作参数：工作电压U1为1000V，工作电流I1为450mA；辅助离子源工作参数：工作电压U2为300V，工作电流I2为200mA，在熔融石英和Si基底上制备Si3N4薄膜；
在熔融石英和Si基底上制备Si3N4薄膜时，膜层厚度为300nm；
步骤3中，采用分光光度计测量石英基底上Si3N4薄膜的可见光-近红外透过率曲线，测量范围为300nm-2500nm；采用红外傅立叶光谱仪测量Si基底上Si3N4薄膜的红外透过率曲线，测量范围为2500nm-20000nm；
步骤3中，采用Lambda900分光光度计测量石英基底上Si3N4薄膜的可见光-近红外透过率曲线；
步骤3中，采用PE红外傅立叶光谱仪测量Si基底上Si3N4薄膜的红外透过率曲线；
步骤5中，采用纳米压痕法测量石英基底上Si3N4薄膜的硬度。
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